Treatment method of 2-chloro-5-chloromethylpyridine production wastewater

A technology of chloromethylpyridine and treatment method, which is applied in the field of treatment of 2-chloro-5-chloromethylpyridine production wastewater, can solve problems that have not been effectively solved, and achieve resource utilization, good industrialization promotion value, and significant Effects of Economic and Environmental Benefits

Active Publication Date: 2022-04-01
BEIJING HUIYU LEBANG ENVIRONMENT PROTECTION TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The treatment of 2-chloro-5-chloromethylpyridine pr

Method used

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  • Treatment method of 2-chloro-5-chloromethylpyridine production wastewater
  • Treatment method of 2-chloro-5-chloromethylpyridine production wastewater

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Effect test

Embodiment 1

[0040] The waste water used in the embodiment is taken from the 2-chloro-5-chloromethylpyridine production waste water (cyclopentadiene route synthesis route) of a chemical enterprise in Gansu. The water quality is as follows in Table 1:

[0041] Table 1 Wastewater Composition

[0042] project color pH COD (mg / L) Cl- (mg / L) Ammonia nitrogen (mg / L) Total nitrogen (mg / L) Inorganic phosphorus (mg / L) other CCMP hydrolysis wastewater Red Brown 0.5 194432 99582 20317 22271 15363 H+: 3.2mol / L CCMP alkaline washing water brown 6-7 158720 24895 203 3421 156 Salt content: 5%

[0043] Such as figure 1 process shown.

[0044] The first step is to remove phosphorus by crystallization and recover trisodium phosphate. Take 20L of CCMP hydrolysis wastewater, add 4.5L of 32% sodium hydroxide, adjust the pH to alkaline, stir evenly, send it to a cooling crystallizer to cool down, crystallize at -5°C for 2h, take out the solid-liquid ...

Embodiment 2

[0052] The used waste water of embodiment 2 is identical with embodiment 1.

[0053] The first step is to remove phosphorus by crystallization and recover trisodium phosphate. Take 20L of CCMP hydrolysis wastewater, add 6.5L of sodium carbonate with a mass fraction of 20% and 2L of 32% sodium hydroxide, adjust the pH to alkaline, stir evenly, send it to a cooling crystallizer to cool down, and crystallize at 0°C for 3 hours , take out the solid-liquid separation, recover and obtain 3.1 kg of trisodium phosphate dodecahydrate, and the filtrate goes to the next step for processing.

[0054] The water quality of the filtrate was tested, and the COD was 78219mg / L, and the COD removal rate was 59.8%; the inorganic phosphorus content was 1020 mg / L, and the removal rate was 93.4%.

[0055] In the second step, high-temperature hydrolysis recovers dimethylamine. Take the filtrate after crystallization and phosphorus removal in the previous step, add 5.5L of sodium hydroxide solution ...

Embodiment 3

[0061] The waste water used in the embodiment is taken from the 2-chloro-5-chloromethylpyridine production waste water (cyclopentadiene route synthesis route) of a chemical enterprise in Shandong. The water quality is as follows in Table 2:

[0062] Table 2

[0063] project color pH COD (mg / L) Cl- (mg / L) Ammonia nitrogen (mg / L) Total nitrogen (mg / L) Inorganic phosphorus (mg / L) other CCMP hydrolysis wastewater Red Brown 0.5 305555 127638 44427 44530 32740 H+: 4.7mol / L CCMP alkaline washing water brown 6-7 93650 18357 283 327 230 Salt content: 3%

[0064] The first step is to remove phosphorus by crystallization and recover trisodium phosphate. Take 20L of CCMP hydrolysis wastewater, add 4.5L of sodium carbonate with a mass fraction of 20% and 4.5L of 32% sodium hydroxide, adjust the pH to alkaline, stir evenly, send it to a cooling crystallizer to cool down, and crystallize at 6°C After 1 hour, the solid-liquid separa...

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Abstract

The invention belongs to the field of pesticide intermediate production wastewater treatment, and discloses a 2-chloro-5-chloromethylpyridine pesticide intermediate wastewater pretreatment method. Comprising the following steps: 1) crystallizing, dephosphorizing and recovering sodium phosphate; 2) carrying out pyrohydrolysis to recover dimethylamine; 3) treating the wastewater by a catalytic wet oxidation technology to remove toxic organic pollutants; and 4) the oxidized effluent is decolored and evaporated, the effluent is evaporated and desalted to obtain a white byproduct sodium chloride, and the evaporated effluent is non-toxic and can be reused for production. By adopting the pretreatment method, the treatment effect is good, resource utilization of the 2-chloro-5-chloromethylpyridine production wastewater can be realized, meanwhile, non-biodegradable substances in the wastewater are reduced, and the biodegradability of the wastewater is improved. The method can effectively solve the problem of stable and up-to-standard discharge of the 2-chloro-5-chloromethylpyridine pesticide intermediate production wastewater, and has obvious environmental benefits, economic benefits and social benefits.

Description

technical field [0001] The invention relates to the technical field of wastewater treatment, in particular to a treatment method for wastewater produced by 2-chloro-5-chloromethylpyridine. Background technique [0002] 2-Chloro-5-chloromethylpyridine (CCMP for short) is an important intermediate for the synthesis of neonicotinoid pesticides such as imidacloprid, acetamiprid, and nitenpyram. At present, most domestic enterprises produce CCMP through the cyclopentadiene ring method synthesis method: add acrolein dropwise to cyclopentadiene to get 5-norbornene-2-aldehyde, and then use toluene as solvent to drop the intermediate Add it to acrylonitrile, potassium hydroxide, and tert-butanol to react to obtain 2-cyanoethyl-5-norbornene-2-aldehyde, which can be cracked to obtain 2-methylene-4-cyanobutyraldehyde; then pass chlorine gas Chlorination, and finally adding phosphorus oxychloride or phosphorus pentachloride with DMF as solvent for ring closure reaction to obtain CCMP. ...

Claims

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Application Information

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IPC IPC(8): C02F9/10C02F101/30C02F101/34C02F101/38C02F103/36
CPCY02W10/37
Inventor 程迪欧云川杨宏伟
Owner BEIJING HUIYU LEBANG ENVIRONMENT PROTECTION TECH CO LTD
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