CN112607939B - Method for recovering cyhalofop-butyl solvent by using continuous extraction method - Google Patents

Method for recovering cyhalofop-butyl solvent by using continuous extraction method Download PDF

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CN112607939B
CN112607939B CN202011387474.8A CN202011387474A CN112607939B CN 112607939 B CN112607939 B CN 112607939B CN 202011387474 A CN202011387474 A CN 202011387474A CN 112607939 B CN112607939 B CN 112607939B
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cyhalofop
extraction tank
tank
butyl
extraction
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CN112607939A (en
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刘继巍
王法强
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Vision Fluorochem (nanjing) Ltd
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Vision Fluorochem (nanjing) Ltd
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/26Treatment of water, waste water, or sewage by extraction
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C02F1/048Purification of waste water by evaporation
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

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  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

The invention discloses a method for recovering a cyhalofop-butyl solvent by using a continuous extraction method, which comprises the following process steps: feeding a waste liquid material; adding xylene; stirring; carrying out liquid separation after standing; the separated solvent is dehydrated, stirred, fractionated and desolventized, and then the recovery of the cyhalofop-butyl solvent can be completed; on the basis of the prior art, the method for recovering the cyhalofop-butyl solvent in the wastewater generated in the production process of the cyhalofop-butyl solvent is provided in a breakthrough manner, and the device is matched to effectively recover the cyhalofop-butyl solvent in the wastewater, so that the production yield of the cyhalofop-butyl solvent is effectively improved, and the economic benefit of the cyhalofop-butyl solvent in industrial production is effectively improved.

Description

Method for recovering cyhalofop-butyl solvent by using continuous extraction method
Technical Field
The invention relates to the technical field of cyhalofop-butyl recovery, in particular to a method for recovering a cyhalofop-butyl solvent by using a continuous extraction method.
Background
Cyhalofop-butyl is the only one species with high safety to rice in aryloxy-phenoxy-propionic acid herbicides, and is mainly used for preventing and removing important grassy weeds.
Disclosure of Invention
The invention provides a method for recovering a cyhalofop-butyl solvent by using a continuous extraction method, aiming at solving the problem that the prior art is lack of a method for recovering cyhalofop-butyl.
The method for recovering the cyhalofop-butyl solvent by using the continuous extraction method comprises the following process steps:
starting a waste liquid feeding pump, opening a feeding valve of the first extraction tank, and closing the waste liquid feeding pump after feeding is complete;
after the waste liquid is fed, starting a discharge valve of a xylene storage tank, starting a discharge pump of the xylene storage tank, and pumping xylene with a preset flow into the first extraction tank;
after the xylene is pumped into the extraction tank, closing a discharge valve of the xylene storage tank, simultaneously closing a discharge pump of the xylene storage tank, and starting the stirring of the first extraction tank;
after stirring, standing for 1-2 h, opening a drainage valve of the first extraction tank, and closing the drainage valve of the first extraction tank after liquid on the lower side of the first extraction tank is drained to a treatment tank;
starting a discharge pump of the first extraction tank, pumping residual solvent in the first extraction tank into the second extraction tank, and closing the discharge pump of the first extraction tank after pumping is completed;
after the feeding of the second extraction tank is finished, starting a discharge pump of an anhydrous calcium chloride storage tank, and pumping a predetermined amount of anhydrous calcium chloride into the second extraction tank;
after the pumping is finished, starting the second extraction tank for stirring, stirring for 20min, and standing for 30 min;
after standing, starting a discharge pump of the second extraction tank, opening a feed valve of the third extraction tank, and closing the discharge pump of the second extraction tank after complete discharge;
and after the feeding is finished, closing a feeding valve of the third extraction tank, and after fractionation, desolventizing the fraction to finish the recovery of the cyhalofop-butyl solvent.
Wherein the predetermined flow rate of the dimethylbenzene is 1-2 m 3 /h。
The waste liquid is waste water mixed with 1-4% of cyhalofop-butyl in mass ratio, and the waste water is remained after a water washing method is utilized in a cyhalofop-butyl production process.
Wherein the fractionation comprises the steps of:
heating the third extraction tank to a first temperature range for distillation, sending the distilled fraction to a xylene storage tank, and measuring the specific gravity of the residual solvent;
stopping distilling when the specific gravity of the residual solvent is 1.2-1.3, and heating the third extraction tank again to a second temperature range;
the distillate distilled in the second temperature range is the crude product of the cyhalofop-butyl.
Wherein the first temperature range is 137-140 ℃.
Wherein the second temperature range is 360-363 ℃.
Wherein the predetermined amount of the anhydrous calcium chloride is 1kg/1m 3.
The invention has the beneficial effects that: on the basis of the prior art, the recovery method of the cyhalofop-butyl solvent in the wastewater generated in the production process of the cyhalofop-butyl solvent is provided in a breakthrough manner, and the device is matched to effectively recover the cyhalofop-butyl solvent in the wastewater, so that the production yield of the cyhalofop-butyl solvent is effectively improved, and the economic benefit of the cyhalofop-butyl solvent in industrial production is effectively improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a process flow diagram of the present invention for recovering cyhalofop-butyl solvent using a continuous extraction process.
FIG. 2 is a schematic diagram of the process steps of the method for recovering cyhalofop-butyl solvent by using a continuous extraction method according to the present invention.
FIG. 3 is a schematic diagram of the process steps of the fractional distillation of the present invention process for recovering cyhalofop-butyl solvent using a continuous extraction method.
FIG. 4 is a schematic diagram of the process steps of the waste liquid treatment of the method for recovering a cyhalofop-butyl solvent using a continuous extraction method according to the present invention.
10-a first extraction tank, 20-a xylene storage tank, 30-a second extraction tank, 40-an anhydrous calcium chloride storage tank, 50-a third extraction tank, 60-a treatment tank, 11-a first extraction tank feeding valve, 12-a waste liquid feeding pump, 13-a first extraction tank drainage valve, 14-a discharge pump, 21-a xylene storage tank discharge valve, 22-a xylene storage tank discharge pump, 31-a second extraction tank discharge pump, 41-an anhydrous calcium chloride storage tank discharge pump, 51-a third extraction tank feeding valve, 61-an aeration tank and 62-an oxidation tank.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
In the description of the present invention, it is to be understood that the terms "length", "width", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships illustrated in the drawings, and are used merely for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention. Further, in the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Referring to fig. 1 to 4, the present invention provides a technical solution:
the method for recovering the cyhalofop-butyl solvent by using the continuous extraction method comprises the following process steps:
s101, starting a waste liquid feeding pump 12, opening a feeding valve 11 of a first extraction tank, and closing the waste liquid feeding pump 12 when feeding is complete;
s102, after the waste liquid feeding is completed, starting a xylene storage tank discharging valve 21, starting a xylene storage tank discharging pump 22, and pumping xylene with a preset flow into the first extraction tank 10;
s103, after finishing the xylene pumping, closing a xylene storage tank discharge valve 21, simultaneously closing a xylene storage tank discharge pump 22, and starting the stirring of the first extraction tank 10;
s104, standing for 1-2 hours after stirring is completed, opening a first extraction tank drainage valve 13, and closing the first extraction tank drainage valve 13 after liquid on the lower side of the first extraction tank 10 is drained to a treatment pool 60;
s105, starting the discharge pump 14 of the first extraction tank 10, pumping the residual solvent in the first extraction tank 10 into the second extraction tank 30, and closing the discharge pump 14 of the first extraction tank 10 after pumping is completed;
s106, after the feeding of the second extraction tank 30 is finished, starting a discharge pump 41 of the anhydrous calcium chloride storage tank, and pumping a predetermined amount of anhydrous calcium chloride into the second extraction tank 30;
s107, after the driving is finished, starting the second extraction tank 30 to stir, stirring for 20min, and standing for 30 min;
s108, after standing, starting a discharge pump 31 of the second extraction tank, opening a feed valve 51 of the third extraction tank, and closing the discharge pump 31 of the second extraction tank after complete discharge;
and S109, after the feeding is finished, closing the feeding valve 51 of the third extraction tank, fractionating, and desolventizing the fraction to finish the recovery of the cyhalofop-butyl solvent.
Further, the preset flow rate of the dimethylbenzene is 1-2 m 3 /h。
Further, the waste liquid is waste water mixed with 1-4% of cyhalofop-butyl in mass ratio, wherein the waste water is remained after a water washing method is utilized in a cyhalofop-butyl production process.
Further, the fractionation comprises the steps of:
s201, heating the third extraction tank 50 to a first temperature range for distillation, sending the distilled fraction to a xylene storage tank 20, and measuring the specific gravity of the residual solvent;
s202, stopping distillation when the specific gravity of the residual solvent is 1.2-1.3, and heating the third extraction tank 50 to a second temperature range again;
and S203, distilling the crude product of the cyhalofop-butyl at the second temperature range.
Further, the first temperature range is 137-140 ℃.
Further, the second temperature range is 360-363 ℃.
Further, the predetermined amount of the anhydrous calcium chloride is 1kg/1m 3.
Further, the discharging the liquid at the lower side of the first extraction tank 10 to the treatment tank 60 includes the following steps:
s301, sending the liquid to an aeration tank 61 of a treatment tank 60 for aeration for 1-2 days;
s302, sending the liquid subjected to aeration treatment to the oxidation pond 62 of the treatment pond 60 for biological oxidation, thereby completing the treatment of the liquid.
Specific example 1:
recovering cyhalofop-butyl production wastewater mixed with 2% of cyhalofop-butyl in a certain batch by detection, starting a waste liquid feeding pump 12, opening a feeding valve 11 of a first extraction tank, and closing the waste liquid feeding pump 12 when feeding is complete; after the waste liquid feeding is completed, starting a xylene storage tank discharging valve 21, starting a xylene storage tank discharging pump 22, and pumping 1m into the first extraction tank 10 3 H xylene; after the xylene is pumped into the extraction tank, closing a discharge valve 21 of the xylene storage tank, closing a discharge pump 22 of the xylene storage tank, and starting the stirring of the first extraction tank 10; after stirring, standing for 1h, opening a first extraction tank drainage valve 13, after liquid on the lower side of the first extraction tank 10 is drained to the treatment tank 60, closing the first extraction tank drainage valve 13, and delivering the liquid to an aeration tank 61 of the treatment tank 60 for aeration for 1 day; the liquid after aeration treatment is sent to an oxidation pond 62 of the treatment pond 60 for biological oxidation, thereby completing the treatment of the liquid; starting the discharge pump 14 of the first extraction tank 10, pumping the residual solvent in the first extraction tank 10 into the second extraction tank 30, and closing the discharge pump 14 of the first extraction tank 10 after pumping is completed; after the feeding of the second extraction tank 30 is completed, starting the discharge pump 41 of the anhydrous calcium chloride storage tank, and pumping a predetermined amount of anhydrous calcium chloride into the second extraction tank 30; after the pumping is finished, starting the second extraction tank 30 for stirring, and standing for 30min after stirring for 20 min; after standing, starting the discharge pump 31 of the second extraction tank, opening the feeding valve 51 of the third extraction tank, and closing the discharge pump 31 of the second extraction tank after discharging completely; after the feeding is finished, the valve is closedA third extraction tank feeding valve 51 for heating the third extraction tank 50 to 140 ℃ for distillation, sending the distilled fraction to the xylene storage tank 20, and measuring the specific gravity of the remaining solvent; stopping distilling when the specific gravity of the residual solvent is 1.2, and heating the third extraction tank to 50-360 ℃; and the fraction is a crude product of cyhalofop-butyl, and the recovery of the cyhalofop-butyl solvent can be completed by desolventizing the fraction.
Specific example 2:
recovering the cyhalofop-butyl production wastewater mixed with 4% of cyhalofop-butyl in mass ratio in a certain batch, starting a waste liquid feeding pump 12, opening a feeding valve 11 of a first extraction tank, and closing the waste liquid feeding pump 12 when the feeding is complete; after the waste liquid feeding is completed, starting a xylene storage tank discharging valve 21, starting a xylene storage tank discharging pump 22, and pumping 2m into the first extraction tank 10 3 H xylene; after the xylene is pumped into the extraction tank, closing a discharge valve 21 of the xylene storage tank, closing a discharge pump 22 of the xylene storage tank, and starting the stirring of the first extraction tank 10; after stirring, standing for 2 hours, opening a first extraction tank drain valve 13, after liquid on the lower side of the first extraction tank 10 is discharged to the treatment tank 60, closing the first extraction tank drain valve 13, and sending the liquid to an aeration tank 61 of the treatment tank 60 for aeration for 2 days; the liquid after aeration treatment is sent to an oxidation pond 62 of the treatment pond 60 to carry out biological oxidation, thereby completing the treatment of the liquid; starting the discharge pump 14 of the first extraction tank 10, pumping the residual solvent in the first extraction tank 10 into the second extraction tank 30, and closing the discharge pump 14 of the first extraction tank 10 after pumping is completed; after the feeding of the second extraction tank 30 is completed, starting the discharge pump 41 of the anhydrous calcium chloride storage tank, and pumping a predetermined amount of anhydrous calcium chloride into the second extraction tank 30; after the pumping is finished, starting the second extraction tank 30 to stir, stirring for 20min, and standing for 30 min; after standing, starting the discharge pump 31 of the second extraction tank, opening the feeding valve 51 of the third extraction tank, and closing the discharge pump 31 of the second extraction tank after discharging completely; after the feeding is completed, the third extraction tank feeding valve 51 is closed, the third extraction tank 50 is heated to 137 ℃ for distillation, the distilled fraction is sent to the xylene storage tank 20, and the specific gravity of the remaining solvent is measured; until the residual solvent has a specific gravity ofStopping distillation when the temperature is 1.3 ℃, and heating the third extraction tank to 50-363 ℃; and the fraction is a crude product of cyhalofop-butyl, and the recovery of the cyhalofop-butyl solvent can be completed by desolventizing the fraction.
On the basis of the prior art, the invention provides a method for recovering cyhalofop-butyl solvent in wastewater generated in the production process of cyhalofop-butyl solvent in a breakthrough manner, and the recovery of the cyhalofop-butyl solvent in the wastewater is effectively finished by utilizing the cooperation of all devices, so that the production yield of the cyhalofop-butyl solvent is effectively improved, and the economic benefit of the cyhalofop-butyl solvent in industrial production is effectively improved.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (7)

1. The method for recovering the cyhalofop-butyl solvent by using the continuous extraction method is characterized by comprising the following process steps of:
starting a waste liquid feeding pump, opening a feeding valve of the first extraction tank, and closing the waste liquid feeding pump when the feeding is complete;
after the waste liquid is fed, starting a discharge valve of a xylene storage tank, starting a discharge pump of the xylene storage tank, and pumping xylene with a preset flow into the first extraction tank;
after the xylene is pumped into the extraction tank, closing a discharge valve of the xylene storage tank, simultaneously closing a discharge pump of the xylene storage tank, and starting the stirring of the first extraction tank;
after stirring, standing for 1-2 h, opening a drainage valve of the first extraction tank, and closing the drainage valve of the first extraction tank after liquid on the lower side of the first extraction tank is drained to a treatment tank;
starting a discharge pump of the first extraction tank, pumping the residual solvent in the first extraction tank into the second extraction tank, and closing the discharge pump of the first extraction tank after pumping is completed;
after the feeding of the second extraction tank is finished, starting a discharge pump of an anhydrous calcium chloride storage tank, and pumping a predetermined amount of anhydrous calcium chloride into the second extraction tank;
after the pumping is finished, starting the second extraction tank for stirring, stirring for 20min, and standing for 30 min;
after standing, starting a discharge pump of the second extraction tank, opening a feed valve of the third extraction tank, and closing the discharge pump of the second extraction tank after complete discharge;
and after the feeding is finished, closing a feeding valve of the third extraction tank, and after fractionation, desolventizing the fraction to finish the recovery of the cyhalofop-butyl solvent.
2. The method for recovering cyhalofop-butyl solvent by using the continuous extraction method as claimed in claim 1, wherein the predetermined flow rate of the xylene is 1-2 m 3 /h。
3. The method for recovering a cyhalofop-butyl solvent by using a continuous extraction method as claimed in claim 1, wherein the waste liquid is waste water mixed with 1-4% by mass of cyhalofop-butyl remaining after a water washing method in a cyhalofop-butyl production process.
4. The method for recovering cyhalofop-butyl solvent using a continuous extraction method as claimed in claim 1, wherein the fractional distillation comprises the steps of:
heating the third extraction tank to a first temperature range for distillation, sending the distilled fraction to a xylene storage tank, and measuring the specific gravity of the residual solvent;
stopping distilling when the specific gravity of the residual solvent is 1.2-1.3, and heating the third extraction tank again to a second temperature range;
the distillate distilled in the second temperature range is the crude product of the cyhalofop-butyl.
5. The method for recovering cyhalofop-butyl solvent by using the continuous extraction method as claimed in claim 4, wherein the first temperature range is 137-140 ℃.
6. The method for recovering a cyhalofop-butyl solvent by a continuous extraction method as claimed in claim 5, wherein the second temperature range is 360-363 ℃.
7. The method for recovering a cyhalofop-butyl solvent using a continuous extraction method as claimed in claim 1, wherein the predetermined amount of the anhydrous calcium chloride is 1kg/1m 3
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WO2010030617A1 (en) * 2008-09-09 2010-03-18 Meadwestvaco Corporation A method of recovering levulinic acid
CN103769056A (en) * 2014-02-07 2014-05-07 中国农业大学 Adsorption and content-detection methods for aryloxy-phenoxy carboxylic acid ester herbicides in water sample and primary metabolites of aryloxy-phenoxy carboxylic acid ester herbicides
CN108585335A (en) * 2018-05-18 2018-09-28 曲阜师范大学 A kind of phenylhydrazine hydrochloride production liquid waste processing and recovery method as resource

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Denomination of invention: A Method for Recovering Cyanoflufen Solvent by Continuous Extraction

Granted publication date: 20220909

Pledgee: Bank of China Limited by Share Ltd. Nanjing Xuanwu sub branch

Pledgor: VISION FLUOROCHEM (NANJING) LTD.

Registration number: Y2024980003265