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Lignin-based dithiocarbamate heavy metal ion capture agent and preparation method

A technology of prime dithiocarbamic acid and prime dithioamino, applied in the treatment of heavy metal-contaminated soil, heavy metal ion wastewater, lignin-based dithiocarbamate heavy metal ion scavenger and preparation field , can solve the problems of high cost of use and restrictions on the large-scale promotion and application of DTC, and achieve the effects of not being prone to secondary pollution, strong heavy metal ion capture ability, and simple use methods

Inactive Publication Date: 2012-11-21
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because the synthesis of traditional DTC requires a large amount of expensive amines such as melamine, diethylenetriamine and other compounds to introduce amino groups, and then react with carbon disulfide, the cost of use remains high. Therefore, the large-scale use of DTC is severely limited. Promote application

Method used

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  • Lignin-based dithiocarbamate heavy metal ion capture agent and preparation method
  • Lignin-based dithiocarbamate heavy metal ion capture agent and preparation method
  • Lignin-based dithiocarbamate heavy metal ion capture agent and preparation method

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Effect test

Embodiment 1

[0039] The operation steps of the preparation method of the lignin-based dithiocarbamate heavy metal ion scavenger are as follows: under normal pressure, take 100g alkali lignin and dissolve it in distilled water to prepare a mixed solution with a mass fraction of 30%, add hydrogen Sodium oxide adjusted the pH of the mixture to 11, and then added H 2 o 2 Oxidant 13.88g, under mechanical stirring (300 r min -1 ) under heating to 90°C, react for 1 hour; add 43.55g of diethylenetriamine, keep the reaction temperature unchanged, then slowly drop in 21.23g of formaldehyde (about 30 minutes to finish dripping, so as not to overflow when the temperature is too high), and stir Under reflux reaction for 5 hours; cool the above solution to room temperature, add an appropriate amount of sodium hydroxide to maintain the pH of the mixed solution = 11, slowly add 52.8g of carbon disulfide dropwise, after the dropwise addition is complete, heat up to 45°C and react for 5 hours, then continu...

Embodiment 2

[0043] The operation steps of the preparation method of the lignin-based dithiocarbamate heavy metal ion scavenger are as follows: under normal pressure, take 100g alkali lignin and dissolve it in distilled water to prepare a mixed solution with a mass fraction of 25%, add hydrogen Potassium oxide was used to adjust the pH to 10, and then 4.08 L of oxygen was introduced into the mixture under mechanical stirring (300 r min -1 ) and heated to 80°C, reacted for 2 hours; added 16.28g of triethylenetetramine, kept the reaction temperature constant, then slowly added 8.33g of formaldehyde (dropped in about 30 minutes, so as not to overflow when the temperature was too high), and stirred reflux for 6 hours; cool the above solution to room temperature, add potassium hydroxide to maintain the pH of the reaction solution = 10, slowly add 19.6 g of carbon disulfide dropwise, wait until the dropwise addition is complete, heat up to 42 ° C and react for 5 hours, continue to add modified A...

Embodiment 3

[0046] The operation steps of the preparation method of the lignin-based dithiocarbamate heavy metal ion scavenger are as follows: under normal pressure, take 100g alkali lignin and dissolve it in distilled water to prepare a mixed solution with a mass fraction of 35%, add hydrogen Potassium oxide and sodium hydroxide were used to adjust the pH to 9, then 10 g of Fenton’s reagent was added, and the mixture was stirred mechanically (300 r min -1 ) to 90°C, and react for 2 hours; add 5.0g of diethylenetriamine and 3.4g of melamine, keep the reaction temperature constant, and then slowly drop in 20.09g of formaldehyde (about 30 minutes to finish dripping, so as not to overheat and overflow ), reflux reaction under stirring for 6 hours; the above solution was cooled to room temperature, and sodium hydroxide was added to adjust the pH=10 of the mixed solution, and a total of 16.87 g of carbon disulfide was slowly added dropwise. , continue to add modifier urea 8.0g, polyacrylamide ...

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Abstract

The invention discloses a preparation method of a lignin-based dithiocarbamate heavy metal ion capture agent. The method comprises the steps of: (1) adding water into lignin and stirring them, adding an alkaline conditioning agent to adjust the pH to 9-11, then adding an oxidizing agent, conducting heating to raise the temperature to 80-90DEG C for reacting for 1-2 hours; (2) adding an amination reagent, maintaining the reaction temperature at 80-90DEG C, then adding formaldehyde to react for 5-6 hours; (3) cooling the solution to room temperature, adjusting the pH value to 10-11, then adding carbon disulfide to perform an esterification reaction for 4-5 hours at 40-45DEG C; and (4) adding a modifier for reacting for 1-2 hours, then carrying out pumping filtration, and then conducting washing 2-3 times with water and absolute ethyl alcohol, thus obtaining a solid product, i.e. the lignin-based dithiocarbamate. The lignin-based dithiocarbamate heavy metal ion capture agent provided in the invention has the advantages of simple preparation process, low production cost, excellent performance, adaptability to treatment of various heavy metal ion polluted wastewater, good stability, and wide applicable range.

Description

technical field [0001] The invention belongs to the technical field of heavy metal ion trapping agents, and in particular relates to a lignin-based dithiocarbamate heavy metal ion trapping agent, a preparation method and its application in the treatment of heavy metal ion wastewater and heavy metal polluted soil. Background technique [0002] Industrial production often produces wastewater containing chromium, nickel, copper, zinc, cadmium, lead, gold, mercury, silver and other heavy metal ions, causing serious pollution to rivers, lakes and seas. Industrial wastewater containing heavy metal ions will cause serious pollution to surface water, groundwater and soil, and cannot be stable in the environment, accumulate in organisms, and easily enter the plant through the root system and be absorbed, inhibiting crop growth and development, and reducing yield , and further enter the human body through the transmission and enrichment of the food chain, causing canceration, deformit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/30C02F1/28C02F1/62
Inventor 葛圆圆
Owner GUANGXI UNIV
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