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Method for treating condensation waste water for producing imidacloprid and resourcized recovering its imidazolidine

A recovery method, imidazolidine technology, applied in the field of condensation wastewater treatment, can solve problems such as waste of resources, failure to be recycled, pollution, etc., and achieve the effect of realizing waste resources

Inactive Publication Date: 2007-03-28
YANCHENG TEACHERS UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the first 6 steps of the above-mentioned production process, each ton of product will produce about 18-20m of waste water 3 , the wastewater is dark red, CODc r It is about 120,000mg / L, the composition is complex, and has no recovery value. Generally, clean production technology is used to reduce the output and evaporation of wastewater for treatment.
In the seventh step, each ton of product will produce about 3~4m 3 Condensation waste water, in which raw materials imidazolidine, methyl ethyl ketone and other organic matter, inorganic salts and CODc r (CODc r About 35,000 mg / L) and a small amount of organic solvents are usually treated by evaporation. Therefore, the condensation wastewater has not been effectively treated, and the imidazolidine has not been recovered. Utilization, waste of resources, and pollution at the same time

Method used

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  • Method for treating condensation waste water for producing imidacloprid and resourcized recovering its imidazolidine
  • Method for treating condensation waste water for producing imidacloprid and resourcized recovering its imidazolidine

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Fill each 20mL (about 15g, dry weight) of JX101 and NDA-7 resins into two adsorption columns with insulation jackets (Ф20×250mm).

[0023] Take 550mL of light yellow condensation wastewater in the production of imidacloprid, filter it, and aerate it for half an hour. Upper column solution COD Cr is 35680mg / L, and the imidazolidine content is 18600mg / L. At room temperature (25°C), 400ml of the upper column solution was passed through the JX101 resin column at a flow rate of 40mL / h. The water produced by the primary adsorption was colorless, and the imidazolidine content dropped to 16800mg / L, COD Cr Drop to 33400mg / L, PH is about 4.

[0024] After neutralizing the first-stage adsorption water with solid NaOH, take 150ml of the upper column liquid and pass it through the NDA-7 resin column at a flow rate of 20mL / h. After the second-stage adsorption water is mixed, the measured imidazolidine content drops to 263mg / L , COD Cr Dropped to 1576mg / L.

[0025] After the seco...

Embodiment 2

[0030] Pack 200mL (about 150g, dry weight) of NDA150 and NDA-7 resins into two adsorption columns (Ф35×500mm) with insulation jackets respectively.

[0031] Take 5L of light yellow condensation wastewater in the production of imidacloprid and filter it, then aerate for half an hour. Upper column solution COD Cr It is 36410mg / L, and the content of imidazolidine is 19100mg / L. At room temperature (25°C), 4.4L of the upper column solution was passed through the NDA150 resin column at a flow rate of 460mL / h. The first-stage adsorption water was colorless, and the measured imidazolidine content dropped to 17900mg / L, COD Cr Drop to 34830mg / L, PH is about 4.

[0032] After the primary adsorption water was neutralized with solid NaOH, 1.6L of the upper column liquid was passed through the NDA-7 resin column at a flow rate of 200mL / h. After the secondary adsorption water was mixed, the imidazolidine content was measured to drop to 963mg / h L, COD Cr Dropped to 3514mg / L.

[0033] Aft...

Embodiment 3

[0038] Pack 300mL (about 225g, dry weight) of NDA150 resin into an adsorption column with a thermal insulation jacket (Ф35×500mm), and 400mL (about 300g, dry weight) of NDA-7 resin are evenly packed into two columns with a thermal insulation jacket In the glass column (Ф35×500mm).

[0039] Take 6L of light yellow condensation wastewater in the production of imidacloprid and filter it, then aerate for half an hour. Upper column solution COD Cr is 35190mg / L, and the imidazolidine content is 18300mg / L. At room temperature (25°C), 4.4L of the upper column liquid was passed through the NDA150 resin column at a flow rate of 400mL / h. Cr Reduced to 34160mg / L, PH is about 4.

[0040] After neutralizing the first-stage adsorption water with solid NaOH to neutrality, take 1.6L of the upper column liquid and pass through two NDA-7 resin columns in turn at a flow rate of 180mL / h, take out the second-stage adsorption water, and measure the COD Cr It is 512mg / L and contains almost no imi...

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Abstract

The invention provides a method of treating condensation waste water in imidacloprid production and recovering imidazole, filtering and aerating the condensation waste water and purifying by ultrahigh cross-linking absorption resin; neutralizing effluent water from primary absorption stage and then passing through macroporous poly-TRIM absorption resin, and distilling, cooling and filtering effluent water from secondary absorption stage and recovering course salts, where the distilled water is recycled in the original process, or aerobically treated to reach the effluent standard and discharged; the macroporous poly-TRIM absorption resin is regenerated by HCl desorption, processed by methanol every multiple batches and able to be repeatedly used; and the eluting liquid is neutralized and frozen so as to separate out imidazole; and the moter liquids are merged many times to recover imidazole; the ultrahigh cross-linking absorption resin is desorbed with methanol and washed with water and then able to be recycled.

Description

Technical field [0001] The invention relates to a method for treating condensation waste water in the production of imidacloprid, a high-efficiency systemic insecticide, specifically, a treatment method for the condensation waste water in the production of imidacloprid and a resource recovery method for imidazolidine. Background technique [0002] At present, the production and synthesis process route of imidacloprid is usually to use cyclopentadiene and acrolein as starting materials, synthesize 2-chloro-5-chloromethylpyridine through multi-steps, and further condense with imidazolidine to obtain 1-(6- Chloro-3-pyridylmethyl)-N-nitroimidazolidine-2-imine (imidacloprid), the specific process is as follows: [0003] [0004] [0005] In the first 6 steps of the above-mentioned production process, each ton of product will produce about 18-20m of waste water 3 , the wastewater is dark red, CODc r It is about 120,000mg / L, the composition is complex, and has no recovery v...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/00C02F1/28C02F1/04C07D233/52
Inventor 费正皓唐伯平周春霖刘总堂张华彬董庆华王彦卿张代臻张根成
Owner YANCHENG TEACHERS UNIV
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