Ethyl polyethylene polyamine polymethacrylate chelating flocculant and preparation method thereof

A technology of poly(ethylene polyamine ethyl ester) and poly(ethylene polyamine) polymethacrylate, applied in the direction of flocculation/precipitation water/sewage treatment, etc. Treatment effect, reduction of volume and moisture content, effect of promoting floc growth

Inactive Publication Date: 2013-05-22
HUNAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] One of the purposes of the present invention is to provide a poly(ethylene polyamine ethyl methacrylate)-based chelating flocculant for the above-mentioned technical problems existing in the existing polymer chelating flocculants. The present invention utilizes methacrylate The quasi-monomer has higher polymerization activity to facilitate the synthesis of polymers with higher relative molecular wei

Method used

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  • Ethyl polyethylene polyamine polymethacrylate chelating flocculant and preparation method thereof
  • Ethyl polyethylene polyamine polymethacrylate chelating flocculant and preparation method thereof
  • Ethyl polyethylene polyamine polymethacrylate chelating flocculant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) According to the molar ratio of ethylenediamine and ethylene oxide is 2:1, add 301g of ethylenediamine into a 1L autoclave, and then add 16.4g of potassium hydroxide with a concentration of 10% by mass Solution, heated to boiling, then passed through 110.1g of ethylene oxide, reacted at 160°C and 0.5MPa for 3h, decompressed to 1333Pa, collected fractions at 102-104.5°C, and obtained 242.5g of N-hydroxyethylethylenediamine;

[0033] (2) Add N-hydroxyethylethylenediamine and 467g of methyl methacrylate obtained in step (1) into a 1.5L reactor with a stirrer, a thermometer and a fractionation tower, and then add 25.9g of calcium hydroxide and 6.5g of phenothiazine, reacted at 70°C for 4h, decompressed to 1333Pa to distill off unreacted methyl methacrylate and N-hydroxyethylethylenediamine, then filtered to remove calcium hydroxide, separated and purified by column chromatography to obtain 347.9 g ethylenediamine ethyl methacrylate;

[0034] (3) Dissolve the ethylened...

Embodiment 2

[0039] (1) According to the molar ratio of ethylenediamine and ethylene oxide of 2.05:1, add 308.5g of ethylenediamine into a 1L high-pressure reactor, and then add 21g of potassium hydroxide with a concentration of 10% by mass Solution, heated to boiling, then passed through 110.1g of ethylene oxide, reacted at 170°C and 0.65MPa for 2.5h, decompressed to 1333Pa, collected fractions at 102-104.5°C, and obtained 243.6g of N-hydroxyethylethylenediamine ;

[0040] (2) Add N-hydroxyethylethylenediamine and 515.4g of methyl methacrylate obtained in step (1) into a 1.5L reactor equipped with a stirrer, thermometer and fractionation tower, and then add 29.5g of calcium hydroxide and 7g of phenothiazine, reacted at 80°C for 3.5h, decompressed to 1333Pa to evaporate unreacted methyl methacrylate and N-hydroxyethylethylenediamine, then filtered to remove calcium hydroxide, and purified by column chromatography to obtain 352.2g ethylenediamine ethyl methacrylate;

[0041] (3) Dissolve ...

Embodiment 3

[0045] (1) According to the molar ratio of ethylenediamine and ethylene oxide is 2.1:1, add 316g of ethylenediamine into a 1L high-pressure reactor, and then add 26g of potassium hydroxide solution with a concentration of 10% by mass , heated to boiling, then passed 110.1g of ethylene oxide, reacted at 180°C and 0.8MPa for 2h, decompressed to 1333Pa, collected fractions at 102-104.5°C, and obtained 243.2g of N-hydroxyethylethylenediamine;

[0046] (2) Add N-hydroxyethylethylenediamine and 561.1g of methyl methacrylate obtained in step (1) into a 1.5L reactor equipped with a stirrer, thermometer and fractionation tower, and then add 31.1g of calcium hydroxide and 7.45g of phenothiazine, reacted at 90°C for 3h, decompressed to 1333Pa to evaporate unreacted methyl methacrylate and N-hydroxyethylethylenediamine, then filtered to remove calcium hydroxide, and purified by column chromatography to obtain 349.5g ethylenediamine ethyl methacrylate;

[0047] (3) Dissolve ethylenediami...

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Abstract

The invention discloses an ethyl polyethylene polyamine polymethacrylate heavy metal chelating flocculant and a preparation method thereof. The method adopts a technical scheme comprising the following steps of: carrying out addition reaction on polyethylene polyamine and ethylene oxide under an alkaline condition to prepare N-ethyl polyethylene polyamine, carrying out ester exchange reaction on N-ethyl polyethylene polyamine and methyl methacrylate in the presence of a catalyst and a polymerization inhibitor to synthesize ethyl polyethylene polyamine methacrylate, synthesizing ethyl polyethylene polyamine polymethacrylate through free radical polymerization, and then performing reaction on ethyl polyethylene polyamine polymethacrylate and carbon disulfide under the alkaline condition to generate the ethyl polyethylene polyamine polymethacrylate chelating flocculant. The ethyl polyethylene polyamine polymethacrylate chelating flocculant overcomes defects such as low relative molecular mass and no functional groups on sectional chain links of high-polymer heavy-metal chelating flocculants. The ethyl polyethylene polyamine polymethacrylate chelating flocculant not only has a good chelating function, but also has an excellent flocculating property, is applicable to the treatment of various heavy metal wastewater, and has broad popularization application value.

Description

technical field [0001] The invention belongs to the field of heavy metal sewage treatment and flocculants, and in particular relates to a polymethacrylic acid polyethylene polyamine ethyl ester-based chelating flocculant integrating heavy metal ion chelation and flocculation functions and a preparation method thereof. Background technique [0002] Heavy metals cannot be degraded by microorganisms, and are easy to accumulate in organisms and cause significant toxic effects. They are persistent pollutants. Once the environment is polluted by heavy metals, it is difficult to control, and the cost of the treatment is quite painful. According to the statistics of the Ministry of Environmental Protection, since 2009, there have been more than 30 serious heavy metal pollution incidents and many blood lead incidents in China, which have seriously threatened the lives of the people. Heavy metal pollution has become one of the hot issues in Chinese society. The prevention and contro...

Claims

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Application Information

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IPC IPC(8): C02F1/56
Inventor 刘立华唐安平周智华曾荣今
Owner HUNAN UNIV OF SCI & TECH
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