Cyanuric acid-based heavy metal chelating flocculant and preparation method thereof

Abstract

The invention belongs to the technical field of heavy metal wastewater treatment, and in particular relates to cyanuric acid-based heavy metal chelating flocculant and a preparation method thereof. In the method, cyanuric acid is adopted as a basic framework; and polyamine is connected to a molecule through epoxy chloropropane, and reacts with carbon disulfide in an alkaline condition to prepare the heavy metal chelating flocculant of which the molecule contains a plurality of branches and a plurality of dithio formate functional groups. The method overcomes the defects that the conventional monofunctional flocculant has small flocculating body, and poor precipitation performance, and when polymeric chelant chelates heavy metals, steric clash is great, and the residual heavy metal ion concentration is difficult to meet the standard and the like. The flocculant has the advantages of simple preparation process, mild condition, easy operation and control, high yield, high raw material utilization, less three waste discharge and environmental protection of technical process, convenient popularization and industrialization realization and suitability for treatment of various types of heavy metal wastewater, such as smelting wastewater, electroplating wastewater, nonferrous metals processing wastewater, mining and beneficiating wastewater, printed circuit board wastewater, battery plants and the like.

Description

technical field

[0001] The invention belongs to the technical field of heavy metal wastewater treatment, in particular to a heavy metal ion treatment agent with multiple branched chains and multiple chelating functional groups, in particular to a cyanuric acid-based heavy metal chelating flocculant and a preparation method thereof. Background technique

[0002] Heavy metal ions such as Hg, Cd, Pb, Cr, As, Cu, and Ni can produce significant toxic effects due to trace amounts, cannot be degraded by microorganisms, and can be enriched thousands of times in higher organisms after being ingested by organisms They can be accumulated and interact strongly with biological macromolecules (such as proteins, enzymes, etc.) to inactivate them, and can also accumulate in certain organs to cause cumulative poisoning. Therefore, heavy metal wastewater is the most serious environmental pollution and harmful to the environment. One of the most harmful industrial wastewater to human beings. ...

Examples

Embodiment 1

[0032] (1) Dissolve 50g cyanuric acid in 2.2L dimethyl sulfoxide to form a solution with a concentration of 2.0% by mass, add it to a 5L reactor with mechanical stirring and reflux condenser, and mix cyanuric acid and epoxy The molar ratio of chloropropane was 1:3.0, and 91mL of epichlorohydrin was slowly added dropwise, the temperature was controlled at 80°C, and the reaction was carried out for 8h.

[0033] (2) According to the molar ratio of epichlorohydrin to triethylenetetramine of 1:1.0, 171.3 mL of triethylenetetramine was slowly added dropwise, and reacted at 60° C. for 5 hours.

[0034] (3) The above reaction mixture is distilled under reduced pressure at 1 mmHg, and the solvent dimethyl sulfoxide is evaporated to obtain a colorless gum, and the dimethyl sulfoxide is collected as a solvent for the next round of reaction;

[0035](4) Add 3.71L of dehydrated ethanol to the jelly obtained in the previous step to form a solution with a mass percent concentration of 10%, a...

Embodiment 2

[0038] (1) 50g cyanuric acid is dissolved in the dimethyl sulfoxide that reclaims in embodiment 1 step (3), is made into the solution that mass percent concentration is 3.5%, joins the reaction that has mechanical stirring and reflux condenser in 5L In the container, according to the molar ratio of cyanuric acid and epichlorohydrin as 1:3.1, slowly add epichlorohydrin 94.2mL dropwise, control the temperature at 90°C, and react for 6h;

[0039] (2) Slowly add 185.9 mL of triethylenetetramine dropwise at a molar ratio of epichlorohydrin to triethylenetetramine of 1:1.05, and react at 70° C. for 5 hours;

[0040] (3) The above reaction mixture is distilled under reduced pressure at 1 mmHg, and the solvent dimethyl sulfoxide is evaporated to obtain a colorless gum, and the dimethyl sulfoxide is collected as a solvent for the next round of reaction;

[0041] (4) The gel obtained in the previous step is added to the solvent separated in Example 1 step (4) and the ethanol for washing...

Embodiment 3

[0044] (1) 50g cyanuric acid is dissolved in the dimethyl sulfoxide that reclaims in embodiment 2 step (3), is made into the solution that mass percent concentration is 5%, joins the reaction that has mechanical stirring and reflux condenser in 5L In the container, according to the molar ratio of cyanuric acid and epichlorohydrin as 1:3.2, slowly add epichlorohydrin 97.2mL dropwise, control the temperature at 70°C, and react for 8h;

[0045] (2) Slowly add 201.0 mL of triethylenetetramine dropwise at a molar ratio of 1:1.1 between epichlorohydrin and triethylenetetramine, and react at 80° C. for 4 hours;

[0046] (3) The above reaction mixture is distilled under reduced pressure at 1 mmHg, and the solvent dimethyl sulfoxide is evaporated to obtain a light yellow gum, and the dimethyl sulfoxide is collected as a solvent for the next round of reaction;

[0047] (4) The gel obtained in the previous step is added to the solvent separated in Example 2 step (4) and the ethanol for w...

technical field

[0001] The invention belongs to the technical field of heavy metal wastewater treatment, in particular to a heavy metal ion treatment agent with multiple branched chains and multiple chelating functional groups, in particular to a cyanuric acid-based heavy metal chelating flocculant and a preparation method thereof. Background technique

[0002] Heavy metal ions such as Hg, Cd, Pb, Cr, As, Cu, and Ni can produce significant toxic effects due to trace amounts, cannot be degraded by microorganisms, and can be enriched thousands of times in higher organisms after being ingested by organisms They can be accumulated and interact strongly with biological macromolecules (such as proteins, enzymes, etc.) to inactivate them, and can also accumulate in certain organs to cause cumulative poisoning. Therefore, heavy metal wastewater is the most serious environmental pollution and harmful to the environment. One of the most harmful industrial wastewater to human beings. ...

Examples

Embodiment 1

[0032] (1) Dissolve 50g cyanuric acid in 2.2L dimethyl sulfoxide to form a solution with a concentration of 2.0% by mass, add it to a 5L reactor with mechanical stirring and reflux condenser, and mix cyanuric acid and epoxy The molar ratio of chloropropane was 1:3.0, and 91mL of epichlorohydrin was slowly added dropwise, the temperature was controlled at 80°C, and the reaction was carried out for 8h.

[0033] (2) According to the molar ratio of epichlorohydrin to triethylenetetramine of 1:1.0, 171.3 mL of triethylenetetramine was slowly added dropwise, and reacted at 60° C. for 5 hours.

[0034] (3) The above reaction mixture is distilled under reduced pressure at 1 mmHg, and the solvent dimethyl sulfoxide is evaporated to obtain a colorless gum, and the dimethyl sulfoxide is collected as a solvent for the next round of reaction;

[0035](4) Add 3.71L of dehydrated ethanol to the jelly obtained in the previous step to form a solution with a mass percent concentration of 10%, a...

Embodiment 2

[0038] (1) 50g cyanuric acid is dissolved in the dimethyl sulfoxide that reclaims in embodiment 1 step (3), is made into the solution that mass percent concentration is 3.5%, joins the reaction that has mechanical stirring and reflux condenser in 5L In the container, according to the molar ratio of cyanuric acid and epichlorohydrin as 1:3.1, slowly add epichlorohydrin 94.2mL dropwise, control the temperature at 90°C, and react for 6h;

[0039] (2) Slowly add 185.9 mL of triethylenetetramine dropwise at a molar ratio of epichlorohydrin to triethylenetetramine of 1:1.05, and react at 70° C. for 5 hours;

[0040] (3) The above reaction mixture is distilled under reduced pressure at 1 mmHg, and the solvent dimethyl sulfoxide is evaporated to obtain a colorless gum, and the dimethyl sulfoxide is collected as a solvent for the next round of reaction;

[0041] (4) The gel obtained in the previous step is added to the solvent separated in Example 1 step (4) and the ethanol for washing...

Embodiment 3

[0044] (1) 50g cyanuric acid is dissolved in the dimethyl sulfoxide that reclaims in embodiment 2 step (3), is made into the solution that mass percent concentration is 5%, joins the reaction that has mechanical stirring and reflux condenser in 5L In the container, according to the molar ratio of cyanuric acid and epichlorohydrin as 1:3.2, slowly add epichlorohydrin 97.2mL dropwise, control the temperature at 70°C, and react for 8h;

[0045] (2) Slowly add 201.0 mL of triethylenetetramine dropwise at a molar ratio of 1:1.1 between epichlorohydrin and triethylenetetramine, and react at 80° C. for 4 hours;

[0046] (3) The above reaction mixture is distilled under reduced pressure at 1 mmHg, and the solvent dimethyl sulfoxide is evaporated to obtain a light yellow gum, and the dimethyl sulfoxide is collected as a solvent for the next round of reaction;

[0047] (4) The gel obtained in the previous step is added to the solvent separated in Example 2 step (4) and the ethanol for w...

Images