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Novel method for recovering trichlorophenol from alkaline wastewater in prochloraz amination process

A technology of trichlorophenol and prochloraz, which is applied in the field of recycling trichlorophenol from alkaline wastewater in the amination process of prochloraz, can solve the problems of reducing sewage treatment effect, sewage station paralysis, death, etc.

Inactive Publication Date: 2020-09-11
江西汇和化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the production process of the prochloraz amination process, there will inevitably be some 2,4,6-trichlorophenol (referred to as "trichlorophenol") that does not fully participate in the reaction. In order to improve the product quality of the aminated product, the production In practice, trichlorophenol is often washed away by alkali washing, and the alkali washing water is directly discharged to the sewage station for bacterial treatment, but trichlorophenol is also a good fungicide, and the wastewater containing trichlorophenol is easily discharged to the sewage station. Kill the bacteria in the sewage station, thereby reducing the sewage treatment effect and even paralyzing the sewage station

Method used

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  • Novel method for recovering trichlorophenol from alkaline wastewater in prochloraz amination process
  • Novel method for recovering trichlorophenol from alkaline wastewater in prochloraz amination process
  • Novel method for recovering trichlorophenol from alkaline wastewater in prochloraz amination process

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Embodiment 1

[0027] A new method for reclaiming trichlorophenol from prochloraz amination process alkaline wastewater comprises the steps:

[0028] (1) Pump the alkaline washing wastewater of the prochloraz amination process into the neutralization reaction kettle, start stirring, and slowly add 30% hydrochloric acid for acidification until white flocculent solids are precipitated, control pH = 3, continue After stirring for 1.5 hours, the solid-liquid separation of the mixed material, the solid is trichlorophenol, and the liquid is waste water I;

[0029] (2) Adopt 55% hydrochloric acid to adjust the pH of the waste water I to 6, add ferrous chloride and hydrogen peroxide, after the oxidation reaction is carried out at 120°C, use 85% sodium hydroxide solution to adjust the pH of the oxidation reaction effluent to 10 , adding sodium hydroxyethylidene diphosphonate, stirring and reacting at 165°C for 2 hours, and filtering to obtain waste water II;

[0030] (3) Add cyclodextrin and polyeth...

Embodiment 2

[0039] A new method for reclaiming trichlorophenol from prochloraz amination process alkaline wastewater comprises the steps:

[0040](1) Pump the alkaline washing wastewater from the prochloraz amination process into the neutralization reactor, start stirring, and slowly add 30% hydrochloric acid for acidification until white flocculent solids are precipitated, control the pH=4, continue After stirring for 2 hours, the solid-liquid separation of the mixed material, the solid is trichlorophenol, and the liquid is waste water I;

[0041] (2) The pH of the waste water I was adjusted to 6 by 60% hydrochloric acid, ferrous chloride and hydrogen peroxide were added, and after the oxidation reaction was carried out at 130° C., the pH of the oxidation reaction effluent was adjusted to 11 by using 90% sodium hydroxide solution. , adding sodium hydroxyethylidene diphosphonate, stirring and reacting at 180°C for 1 to 3 hours, and filtering to obtain waste water II;

[0042] (3) Add cyc...

Embodiment 3

[0051] A new method for reclaiming trichlorophenol from prochloraz amination process alkaline wastewater comprises the steps:

[0052] (1) Pump the alkaline washing wastewater of the prochloraz amination process into the neutralization reaction kettle, start stirring, and slowly add 30% hydrochloric acid for acidification until white flocculent solids are precipitated, control pH = 3, continue After stirring for 1 hour, the solid-liquid separation of the mixed material, the solid is trichlorophenol, and the liquid is waste water I;

[0053] (2) The pH of waste water I using 50% hydrochloric acid is adjusted to 5, ferrous chloride and hydrogen peroxide are added, after the oxidation reaction is carried out at 110° C., the pH of the oxidation reaction effluent is adjusted to 9 using 80% sodium hydroxide solution , adding sodium hydroxyethylidene diphosphonate, stirring and reacting at 150°C for 1 hour, and filtering to obtain waste water II;

[0054] (3) Add cyclodextrin and po...

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Abstract

The invention belongs to the technical field of wastewater treatment, and particularly relates to a novel method for recovering trichlorophenol from alkaline wastewater in a prochloraz amination process. The method comprises the following steps: (1) acidifying alkaline washing wastewater in the prochloraz amination process, and carrying out solid-liquid separation to obtain solid trichlorophenol and a liquid being wastewater I; (2) adjusting the pH value of the wastewater I to 5-6, adding ferrous chloride and hydrogen peroxide, performing an oxidation reaction, adjusting the pH value of oxidation reaction effluent to 9-11, adding 1-hydroxyethanediphosphonic acid sodium salt, stirring for reaction, and filtering to obtain wastewater II; (3) under a stirring condition, adding an ethanol solution of cyclodextrin and polyethyleneimine into the wastewater II, standing, separating out the obtained crystal, and filtering to obtain wastewater III; and (4) adjusting the pH value of the wastewater III to 6-9, and carrying out electrodialysis treatment. The method provided by the invention fully realizes low-cost resource utilization of the alkaline wastewater in the prochloraz amination process.

Description

technical field [0001] The invention belongs to the technical field of waste water treatment, and in particular relates to a new method for recovering trichlorophenol from alkaline waste water in the amination process of prochloraz. Background technique [0002] Prochloraz (Prochloraz), the chemical name is N-propyl-N-(2,4,6-trichlorophenoxyethyl)-1H-imidazole-1-carboxamide, was established by British BootsCo., Ltd. in 1974 Synthesized in 1977, a broad-spectrum imidazole-based high-altitude fungicide introduced to the market in 1977, it works by inhibiting the biosynthesis of sterols, and has a good control effect on various pathogens of rice, fruits and cereals. [0003] At present, domestic manufacturers all adopt the etherification of 2,4,6-trichlorophenol and dichloroethane in sodium hydroxide, followed by amination, acyl chloride and condensation to produce prochloraz. The production process is basically the same. The technological process is as follows: use 2,4,6-tric...

Claims

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Application Information

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IPC IPC(8): C02F9/06C10L5/46C07C37/86C07C37/82C07C37/68C07C39/32C07D233/56C04B7/24C04B7/02C04B7/44C02F101/20C02F101/30C02F103/36
CPCC02F9/00C10L5/46C07C37/86C07C37/82C07C37/68C07D233/56C04B7/24C04B7/02C04B7/44C02F1/66C02F1/722C02F1/001C02F1/4693C02F1/38C02F2101/30C02F2101/203C02F2103/36C07C39/32Y02E50/30Y02E50/10Y02P40/10
Inventor 尹旺华韩井卫曾小明
Owner 江西汇和化工有限公司
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