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A kind of preparation method of n-dithioformyl-n,n-sodium diacetate chelating agent

A technology of dithioformic acid and sodium diacetate, which is applied in chemical instruments and methods, organic chemistry, water/sludge/sewage treatment, etc., and can solve the problems of affecting the use effect and low grafting rate of dithioformic acid groups , achieve the effects of fast sedimentation speed, improved chelation ability, and coarse flocs

Active Publication Date: 2019-12-17
HUNAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Prepare this chelating agent at present and all synthesize under alkali presence with iminodiacetic acid (sodium) and carbon disulfide, owing to be subjected to the influence of molecular structure and group size, the grafting rate of dithioformic acid group is not high (generally in 60%) Below), which affects its use effect

Method used

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  • A kind of preparation method of n-dithioformyl-n,n-sodium diacetate chelating agent
  • A kind of preparation method of n-dithioformyl-n,n-sodium diacetate chelating agent
  • A kind of preparation method of n-dithioformyl-n,n-sodium diacetate chelating agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Take 9.86g of iminodiacetonitrile with a mass fraction of 96.5% and add it to a 250mL three-necked flask with mechanical stirring, reflux condenser and dropping funnel, then add 98.6g of ethanol, stir well, and then add the mass fraction 4.38g of sodium hydroxide of 96.0%, then 6.2mL of carbon disulfide with a mass fraction of 99.0% was added dropwise within 60min at room temperature, then the reaction was continued at room temperature for 3h, and then the temperature was raised to 60°C to continue the reaction for 1h;

[0030] (2) The mixture obtained in step (1) was rotary evaporated at 60°C and -0.095MPa until no solvent dripped out, and 18.97 g of brown sticky matter was obtained; 89.5 g of ethanol collected by rotary evaporation was used for the next round of reaction;

[0031] (3) Transfer the brown viscous matter obtained in step (2) into a 500mL two-necked bottle with mechanical stirring and a condenser tube followed by an airway tube, add 284.6g of distilled...

Embodiment 2

[0036] (1) Get 9.86g mass fraction and be that the iminodiacetonitrile of 96.5% joins in the three-necked bottle of 250mL band mechanical stirring, reflux condenser and dropping funnel, then adds the ethanol 89.5g that embodiment 1 collects, adds again 28.8g of ethanol, fully stirred evenly, then added 4.58g of sodium hydroxide with a mass fraction of 96.0%, then added dropwise 6.5mL of carbon disulfide with a mass fraction of 99.0% within 50min at room temperature, and then continued the reaction at room temperature for 2.5h, Then the temperature was raised to 50° C. to continue the reaction for 2 h;

[0037] (2) The mixture obtained in step (1) was rotary evaporated at 60°C and -0.095MPa until no solvent dripped out to obtain 19.04 g of brown viscous substance; 106.4 g of ethanol collected by rotary evaporation was used for the next round of reaction;

[0038] (3) Transfer the brown viscous matter obtained in step (2) into a 500mL two-necked bottle with a mechanical stirrer ...

Embodiment 3

[0041] (1) get 9.86g mass fraction and be that the iminodiacetonitrile of 96.5% joins in the three-necked flask of 250mL band mechanical stirring, reflux condenser and dropping funnel, then adds the ethanol 106.4g that embodiment 2 collects, adds again 41.5g of ethanol, fully stirred evenly, then add 4.79g of sodium hydroxide with a mass fraction of 96.0%, then dropwise add 6.8mL of carbon disulfide with a mass fraction of 99.0% within 40min at room temperature, then continue the reaction at room temperature for 2h, then Raise the temperature to 50°C and continue the reaction for 1.5h;

[0042] (2) The mixture obtained in step (1) was rotary evaporated at 60°C and -0.095MPa until no solvent dripped out to obtain 18.74 g of brown viscous substance; 132.2 g of ethanol collected by rotary evaporation was used for the next round of reaction;

[0043] (3) Transfer the brown viscous matter obtained in step (2) into a 500mL two-necked bottle with mechanical stirring and a condenser t...

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Abstract

The invention relates to a preparation method of an N-dithioformyl-N,N-sodium diacetate chelating agent. The preparation method comprises the following steps: firstly, carrying out substitution reaction on iminodiacetonitrile, carbon disulfide and alkali in an organic solvent, so as to introduce dithioformyl into a molecule; then adding the alkali to hydrolyze and transform cyano to prepare the N-dithioformyl-N,N-sodium diacetate chelating agent. According to the preparation method provided by the invention, the grafting rate of the dithioformyl in the molecule of a product is remarkably improved, so that the chelating and flocculation capability of the product is improved; produced floc is large and the sedimentation rate is rapid. The preparation method provided by the invention has theadvantages of relatively simple flow, relatively moderate technological conditions and easiness for operation and control; in a technological process, less pollution is generated and a process is environmentally friendly; the preparation method has relatively good popularization and application value.

Description

technical field [0001] The invention relates to the field of heavy metal wastewater treatment, in particular to a preparation method of N-dithioformyl-N,N-sodium diacetate chelating agent. Background technique [0002] With the rapid development of industrial and agricultural production, industries involving heavy metals are increasing, such as mineral mining, smelting and processing, electroplating and surface finishing, metal corrosion and anti-corrosion, textile printing and dyeing, electronic manufacturing and mechanical processing, paint, new energy With the production of new materials, pesticides, fertilizers and daily chemicals, etc., there will be a large amount of wastewater containing various heavy metal ions, such as copper, mercury, nickel, zinc, cadmium, manganese, chromium, lead, arsenic, Thallium, antimony, cobalt, etc. These heavy metals have caused serious harm to human health and the environment due to their high toxicity and non-biodegradable properties. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C333/14C02F1/54C02F1/62C02F101/20
CPCC02F1/54C02F1/62C02F2101/20C07C333/14
Inventor 刘立华刘一达叶小倩王群蒋甜甜黄金美
Owner HUNAN UNIV OF SCI & TECH