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Preparation method of polyepichlorohydrin-ethanediamine decolorizing agent

A polyepichlorohydrin and epichlorohydrin technology, applied in the direction of flocculation/sedimentation water/sewage treatment, etc., can solve the problem of high treatment cost, and achieve the effect of improving the conversion rate, wide application range and good stability

Inactive Publication Date: 2014-01-01
SHANDONG JIANZHU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the disadvantages of traditional flocculants such as combined use with coagulant aids and high processing costs, the present invention provides a method for preparing polyepichlorohydrin-ethylenediamine decolorizer, and the prepared polyepichlorohydrin-ethylenediamine The flocculant has high molecular weight, good decolorization effect and stable performance

Method used

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  • Preparation method of polyepichlorohydrin-ethanediamine decolorizing agent

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Take 24mL of liquid paraffin in a 250mL four-necked round-bottomed flask equipped with a stirrer, thermometer and reflux condenser, place the flask in an ice-water bath, control the temperature at 8°C, and feed a flow rate of 0.5m into the flask. 3 Nitrogen for 15 minutes per hour, then weigh 6.02 g of ethylenediamine and add it to the round bottom flask (the mass ratio of ethylenediamine to liquid paraffin is 1:3), open the cooling water of the reflux condenser, and stir at a G value of 150 S -1 While stirring, the temperature was raised to 25 °C, and 18.56 g of epichlorohydrin (the molar ratio of epichlorohydrin to ethylenediamine was 2:1) was slowly added dropwise with a separatory funnel for addition reaction, and the dropping time was 2.5 hours. After the dropwise addition, continue to stir for 60 minutes; then lower the temperature to below 15°C, and add a trimethylamine crosslinking agent with a mass percentage concentration of 33% according to the molar ratio of ...

Embodiment 2

[0020] Take 48mL of liquid paraffin in a 250mL four-neck round bottom flask, place the flask in an ice-water bath, control the temperature at 5°C, and feed a flow rate of 0.5m into the flask. 3 Nitrogen per hour for 20 minutes, then weigh 12.05 g of ethylenediamine and add it to the round bottom bottle, open the cooling water of the reflux condenser, and stir at a G value of 200 S -1 While stirring, the temperature was raised to 20 ° C, and 18.57 g of epichlorohydrin (the molar ratio of epichlorohydrin to ethylenediamine was 1:1) was slowly added dropwise with a separatory funnel for addition reaction, and the dropping time was 2 hours. Continue to stir for 70 minutes after the dropwise addition; then lower the temperature to 15°C, add 33% trimethylamine crosslinking agent according to the molar ratio of trimethylamine and epichlorohydrin 1:1.5; raise the temperature to 90°C again, and keep the constant temperature React for 5 hours, filter the obtained product to obtain a sol...

Embodiment 3

[0023] Take 96mL of liquid paraffin in a 250mL four-necked round bottom flask, place the flask in an ice-water bath, control the temperature at 0°C, and feed a flow rate of 0.5m into the flask. 3 Nitrogen per hour for 18 minutes, then weigh 24.1 g of ethylenediamine and add it to the round bottom bottle, open the cooling water of the reflux condenser, and stir at G value of 250 S -1 While stirring, the temperature was raised to 23 ° C, and 18.57 g of epichlorohydrin (the molar ratio of epichlorohydrin to ethylenediamine was 1:2) was slowly added dropwise with a separatory funnel for addition reaction, and the dropping time was 3 hours. Continue to stir for 90 minutes after the dropwise addition; then lower the temperature to 15°C, add 33% trimethylamine crosslinking agent according to the molar ratio of trimethylamine and epichlorohydrin 1:1.5; raise the temperature to 87°C again, React for 5 hours, filter the obtained product to obtain a solid product, wash with toluene 2-3 t...

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Abstract

The invention discloses a preparation method of a polyepichlorohydrin-ethanediamine decolorizing agent. The preparation method comprises the following steps: (1), taking and placing liquid paraffin in a four-port round bottom with a stirrer, a thermometer and a reflux condenser, and controlling the temperature to 0 DEG C-8 DEG C; (2), introducing nitrogen gas in the liquid paraffin, adding ethidene diamine in a container, heating up while stirring, controlling the temperature to 20 DEG C-25 DEG C, and slowly dropwise adding polyepichlorohydrin to carry out addition reaction; (3), continuously stirring for thermal reaction after dropwise adding chloropropane, and cooling the temperature to 15 DEG C; (4), taking 33% trimethylamine as a cross-linking agent to add into liquor, and reacting for 5 hours at 85 DEG C-90 DEG C; (5), cleaning a solid product by methylbenzene, cleaning by alcohol and water, vacuum-drying at 60 DEG C and grinding to obtain polyepichlorohydrin-ethanediamine. According to the preparation method, polyepichlorohydrin-ethanediamine is prepared by using polyepichlorohydrin and ethanediamine as materials and introducing a small amount of trimethylamine cross-linking agent, and has the advantages of high molecular weight, good stability, good decolorizing effect and the like.

Description

technical field [0001] The invention relates to a method for preparing an organic polymer flocculant polyepichlorohydrin-ethylenediamine, belonging to the field of flocculant preparation. Background technique [0002] my country discharges a large amount of industrial wastewater and domestic sewage every year, of which dye wastewater and printing and dyeing wastewater account for a considerable proportion, and the resulting ecological environment damage and economic losses are immeasurable. Therefore, the purification and treatment of printing and dyeing wastewater has become a key issue restricting the survival and sustainable development of the current printing and dyeing industry. [0003] Dye wastewater and printing and dyeing wastewater are characterized by complex components, high concentration, high chroma, many refractory substances, and water-soluble organic substances that are biologically toxic or carcinogenic, teratogenic, and mutagenic. At present, among the tr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/10C02F1/56
Inventor 孙翠珍孙玉林张志斌张彦浩武道吉董芳张晓蕊邹彦江
Owner SHANDONG JIANZHU UNIV
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