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Ethylenediamine-based heavy metal chelating agent and preparation method thereof

A heavy metal chelating agent, ethylenediamine-based technology, applied in chemical instruments and methods, water/sludge/sewage treatment, organic chemistry, etc., can solve the problem that the concentration of heavy metal ions is difficult to meet the standard discharge, and is not suitable for large-flow heavy metal wastewater treatment, It is unfavorable for floc growth and other problems, and achieves the effects of easy promotion, convenient storage and transportation, and good flocculation and sedimentation performance

Inactive Publication Date: 2013-08-07
HUNAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The second type of method is expensive and not suitable for the treatment of heavy metal wastewater with large flows
Although monoaminodithioformic acid-based small molecule chelating agents have strong chelating ability, the flocs formed are small and have poor settling performance, and they need to be maintained in an appropriate excess to achieve better results; while polymer chelating agents have better flocculation performance, but the large steric hindrance makes it difficult to discharge the residual heavy metal ion concentration; small molecules containing multifunctional groups can combine the same heavy metal ion with chelating groups from different chelating agent molecules to form macromolecular chelation matter, thereby forming large flocs and improving the sedimentation effect, but there are also some chelating groups that are restricted by the formed chelates when forming large flocs, resulting in space mismatch, so that the microflocs carry some Negative charge is not conducive to the further growth of flocs

Method used

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  • Ethylenediamine-based heavy metal chelating agent and preparation method thereof
  • Ethylenediamine-based heavy metal chelating agent and preparation method thereof
  • Ethylenediamine-based heavy metal chelating agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Add 0.1L ethylenediamine and 2L absolute ethanol to a 10L reactor with mechanical stirring and reflux condenser, then add 244g of granular or flaky solid NaOH with a mass percentage of 96%, and stir Add 362mL of carbon disulfide dropwise, and control the addition rate to raise the temperature of the system to 40-45°C naturally;

[0033] (2) After adding carbon disulfide, add 0.88g of hydroquinone and continue the reaction for 1h;

[0034] (3) Filtration, the filter cake was washed with absolute ethanol, and vacuum-dried to constant weight at 40°C to obtain a light yellow powder, i.e. the product, with a yield of 87.19%, and its sulfur content was determined to be 52.35%;

[0035] After determination, the mass percentage of each component in the product is: the compound content of structural formula (I) is 99.31%; the antioxidant content is 0.13%; the sulfur-containing compound content is 0.51%; the alkali content is 0.05%.

[0036] (4) reclaim step (3) gained filtr...

Embodiment 2

[0040] (1) Add 0.1L of ethylenediamine and the filtrate collected in step (4) of Example 1 to a 10L reactor with mechanical stirring and a reflux condenser, supplement absolute ethanol to 2.5L, and then add 244g mass percent Granular or flaky solid NaOH with a content of 96%, add 345.6mL of carbon disulfide dropwise under stirring, and control the adding speed so that the system naturally heats up to 40-45°C;

[0041] (2) After adding carbon disulfide, add 1.32g of hydroquinone and continue the reaction for 1.5h;

[0042] (3) Filtration, the filter cake was washed with absolute ethanol, and vacuum-dried to constant weight at 40°C to obtain a light yellow powder, i.e. the product, with a yield of 98.54%, and its sulfur content was determined to be 53.11%;

[0043] After determination, the mass percentages of each component in the product are: the compound content of structural formula (I) is 99.05%; the antioxidant content is 0.19%; the sulfur-containing compound content is 0.6...

Embodiment 3

[0046] (1) Add 0.1L of ethylenediamine and the filtrate collected in step (4) of Example 2 to a 10L reactor with mechanical stirring and a reflux condenser, supplement absolute ethanol to 3.0L, and then add 244g mass percent Granular or flaky solid NaOH with a content of 96%, add 362mL of carbon disulfide dropwise under stirring, control the adding speed to make the system naturally warm up to 40-45°C;

[0047] (2) After adding carbon disulfide, add 1.76g of hydroquinone and continue the reaction for 2h;

[0048] (3) Filtration, the filter cake was washed with absolute ethanol, and vacuum-dried to constant weight at 40°C to obtain a light yellow powder, i.e. the product, with a yield of 99.07%, and its sulfur content was determined to be 53.31%;

[0049] After determination, the mass percentage of each component in the product is: the compound content of structural formula (I) is 98.53%; the antioxidant content is 0.25%; the sulfur-containing compound content is 1.15%; the alk...

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Abstract

The invention belongs to the technical field of removal, purification and entrapment of heavy metal ions in a water body, and in particular relates to an ethylenediamine-based heavy metal chelating agent and a preparation method thereof. The ethylenediamine-based heavy metal chelating agent is prepared by directly reacting ethylenediamine, carbon disulfide and solid alkali in absolute ethyl alcohol or a mixed solvent consisting of absolute ethyl alcohol and diethyl ether in a certain volume ratio. The method overcomes the defect of steric effect of polymer chains when the conventional polymeric chelating agent chelates the heavy metal ions, and also overcomes the defect that floccules have excessive negative charge to obstruct the further growth of the floccules because of mismatched space of chelation groups of small molecules with multiple functional groups. The product is solid powder, has high stability and is convenient to store and transport. The method has the advantages of simple synthetic process, mild reaction conditions, easy operation and control, high reaction speed, high efficiency, recyclable solvent, high utilization rate of raw materials, less discharge of three wastes, environmental-friendly technical process, conventional equipment and easy industrial production.

Description

technical field [0001] The invention belongs to the technical field of removing, purifying or trapping heavy metal ions in water bodies, and in particular relates to an ethylenediamine-based heavy metal chelating agent and a preparation method thereof. Background technique [0002] Heavy metal pollution refers to the environmental pollution caused by elements with significant biological toxicity such as Hg, Cd, Pb, Cr, and As, and general heavy metals with certain toxicity, such as Zn, Cu, Co, Ni, Sn and other elements and their compounds. It has the following characteristics: ①A small amount can produce significant toxic effects. Generally, heavy metals can produce toxic effects in the range of 1.0-10mg / L, and the range of significant toxicity is 0.001-0.1mg / L; ②It cannot be degraded by microorganisms. On the contrary, some heavy metals Under the action of microorganisms, it will be transformed into more toxic metal-organic substances, such as mercury into alkylmercury; ③ A...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C333/16C02F1/62
Inventor 刘立华令玉林吴俊曾荣今
Owner HUNAN UNIV OF SCI & TECH
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