CN101700926A - Treatment method of waste liquid of imidazolone type herbicides - Google Patents

Treatment method of waste liquid of imidazolone type herbicides Download PDF

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Publication number
CN101700926A
CN101700926A CN200910230282A CN200910230282A CN101700926A CN 101700926 A CN101700926 A CN 101700926A CN 200910230282 A CN200910230282 A CN 200910230282A CN 200910230282 A CN200910230282 A CN 200910230282A CN 101700926 A CN101700926 A CN 101700926A
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waste liquid
imidazolone type
type herbicides
hydrogen peroxide
autoclave
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CN101700926B (en
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张运林
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Abstract

The invention particularly relates to a treatment method of waste liquid of imidazolone type herbicides. The method comprises the following steps of: (1), leading the waste liquid of the imidazolone type herbicide into an enclosed high-pressure autoclave, wherein eight ultrasonic generators are uniformly distributed around the outside of the high-pressure autoclave; (2), leading hydrogen peroxide into the high-pressure autoclave until the concentration of the hydrogen peroxide in the waste liquid reaches 0.05-0.1 mol/L, then adding sodium hydroxide accounting for 2-5wt% of the waste liquid, raising temperature to 140-160 DEG C, starting the ultrasonic generator with the frequency of 30-45KHz and reacting for 8-12 hours to obtain the reaction liquid. The processing method has the advantages of high decomposition efficiency, mild reaction conditions, recyclable reaction products and can eliminate pollution to the environment.

Description

The treatment process of waste liquid of imidazolone type herbicides
Technical field
The present invention relates to a kind of treatment process of waste liquid of imidazolone type herbicides, relate in particular to a kind of treatment process of waste liquid of imidazolone type herbicides.
Background technology
Imidazolinone herbicide is the another class inhibitor of acetolactate synthetase class weedicide that American Cyanamid Company released behind sulfonylurea herbicide in phase early 1980s, and this class herbicidal activity is higher, and selectivity is strong, can prevent and kill off perennial weeds.Main imidazoles nicotinic acid (imazapyr), miaow barkite (imazamethabez), imazaquin (imazaquin), imazethapyr (imazethapyr) product.
The said products in process of production, because the existence of the isomers of its no weeding activity in solvability of itself and the production process, the imidazolone type organic compound that contains 8%~20% difficult degradation in the waste liquid of gained, cause great difficulty for the later stage wastewater treatment, and cause wastage of material, improved production cost.
Summary of the invention
The object of the present invention is to provide a kind of treatment process of waste liquid of imidazolone type herbicides, have the decomposition efficiency height, reaction conditions gentleness, the advantage of the recyclable utilization of reaction product.
The invention discloses a kind of treatment process of waste liquid of imidazolone type herbicides, it is characterized in that comprising the steps
(1) in enclosed autoclave, feeds waste liquid of imidazolone type herbicides, be evenly equipped with eight ultrasonic generators around the outside of described autoclave;
(2) feed hydrogen peroxide in the autoclave, make the concentration of hydrogen peroxide in waste liquid reach 0.05~0.1mol/L, add the sodium hydroxide that accounts for waste liquid 2-5wt% again, be warming up to 140~160 ℃, open ultrasonic generator, the frequency of ultrasonic generator is 30~45KHz reaction 8h~12h, gets reaction solution.
Contain compound 2 and compound 1 in the waste liquid of imidazolone type herbicides, compound 2 is the isomers of compound 1.
Figure G2009102302823D0000021
Wherein: R is a hydrogen or alkyl;
The oxidative degradation mechanism of waste liquid of imidazolone type herbicides of the present invention is as follows:
Figure G2009102302823D0000022
Wherein: R is a hydrogen or alkyl.
Method of the present invention can make the tetrahydroglyoxaline ring open loop in the imidazolinone herbicide structure generate corresponding compounds 3 (2,3-dinicotinic acid or derivatives thereof), be under the condition of ultrasonic stimulation of 30~45KHz in frequency, reactivity can reach 70%~90%, it can reclaim the raw material of producing as imidazolinone herbicide and utilize, or its further oxidative degradation reached wastewater discharge standard, thereby eliminated the pollution that a large amount of imidazolone type discharging of waste liquid cause to environment, and can effectively reduce production costs.Reaction solution in the treatment process of waste liquid of imidazolone type herbicides of the present invention reclaims 2 after treatment, and 3-dinicotinic acid or further oxidative degradation reach wastewater discharge standard.Treatment process of the present invention has the decomposition efficiency height, reaction conditions gentleness, the advantage of the recyclable utilization of reaction product.
Embodiment
Below in conjunction with specific embodiment essentiality content of the present invention is further described.
Embodiment 1
In the waste liquid of imidazolone type herbicides of this enforcement, contain weight percent and be 10% imidazolone type organic compound.
Its treatment process is: at room temperature feed above-mentioned waste liquid of imidazolone type herbicides 1000L in enclosed autoclave, be evenly equipped with eight ultrasonic generators around the outside of described autoclave; Interior 30% (V/V) hydrogen peroxide that feeds of autoclave makes the concentration of hydrogen peroxide in waste liquid reach 0.06mol/L, adds and the sodium hydroxide that accounts for waste liquid 2wt% again, is warming up to 140 ℃, opens ultrasonic generator, regulates vibrational frequency 30KHz, and reaction 12h gets reaction solution.
Reaction solution in the treatment process of waste liquid of imidazolone type herbicides of the present invention reclaims 2 after treatment, and 3-dinicotinic acid or further oxidative degradation reach wastewater discharge standard.
After tested: the ratio that imidazolone compound is converted into the corresponding pyridine dioctyl phthalate is 75%.
Embodiment 2
It is 15% imidazolone type organic compound that the waste liquid of imidazolone type herbicides of this enforcement contains weight percent.
At room temperature in enclosed autoclave, feed above-mentioned waste liquid of imidazolone type herbicides 1000L, be evenly equipped with eight ultrasonic generators around the outside of described autoclave; The interior 20wt% hydrogen peroxide that feeds of autoclave makes the concentration of hydrogen peroxide in waste liquid reach 0.1mol/L, adds again and the sodium hydroxide that accounts for waste liquid 5wt%,, be warming up to 160 ℃, open ultrasonic generator, regulate vibrational frequency 40KHz, reaction 8h gets reaction solution.
Reaction solution in the treatment process of waste liquid of imidazolone type herbicides of the present invention reclaims 2 after treatment, and 3-dinicotinic acid or further oxidative degradation reach wastewater discharge standard.
After tested: the ratio that imidazolone compound is converted into the corresponding pyridine dioctyl phthalate is 88%.
Embodiment 3
It is 20% imidazolone type organic compound that the waste liquid of imidazolone type herbicides of this enforcement contains weight percent.
At room temperature in enclosed autoclave, feed above-mentioned waste liquid of imidazolone type herbicides 1000L, be evenly equipped with eight ultrasonic generators around the outside of described autoclave; Interior 30% (V/V) hydrogen peroxide that feeds of autoclave makes the concentration of hydrogen peroxide in waste liquid reach 0.08mol/L, adds and the sodium hydroxide that accounts for waste liquid 4wt% again, is warming up to 150 ℃, opens ultrasonic generator, regulates vibrational frequency 45KHz, and reaction 8h gets reaction solution.
Reaction solution in the treatment process of waste liquid of imidazolone type herbicides of the present invention reclaims 2 after treatment, and 3-dinicotinic acid or further oxidative degradation reach wastewater discharge standard.
After tested: the ratio that imidazolone compound is converted into the corresponding pyridine dioctyl phthalate is 85%.

Claims (1)

1. the treatment process of a waste liquid of imidazolone type herbicides is characterized in that comprising the steps:
(1) in enclosed autoclave, feeds waste liquid of imidazolone type herbicides, be evenly equipped with eight ultrasonic generators around the outside of described autoclave;
(2) feed hydrogen peroxide in the autoclave, make the concentration of hydrogen peroxide in waste liquid reach 0.05~0.1mol/L, add the sodium hydroxide that accounts for waste liquid 2-5wt% again, be warming up to 140~160 ℃, open ultrasonic generator, the frequency of ultrasonic generator is 30~45KHz reaction 8h~12h, gets reaction solution.
CN2009102302823A 2009-11-20 2009-11-20 Treatment method of waste liquid of imidazolone type herbicides Expired - Fee Related CN101700926B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101935123A (en) * 2010-09-01 2011-01-05 合肥星宇化学有限责任公司 Method for recycling waste acid and waste residues in production of herbicide oxadiazon
CN105984916A (en) * 2015-02-10 2016-10-05 沈智奇 High-pressure, multiple-frequency and multiple-direction ultrasonic sewage purifier
CN109956537A (en) * 2019-03-26 2019-07-02 河北科技大学 A kind of processing method of the waste water containing acetone cyanohydrin
CN113003852A (en) * 2020-11-13 2021-06-22 四川全息生态环境技术产业有限公司 Ultrasonic wave and H2O2And micro-channel advanced oxidation method and device

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000288495A (en) * 1999-04-01 2000-10-17 Nomura Micro Sci Co Ltd Cleaning method
JP2006035140A (en) * 2004-07-28 2006-02-09 Maywa Co Ltd Method for decomposing agricultural chemical in waste water
CN101307030A (en) * 2008-06-06 2008-11-19 山东潍坊润丰化工有限公司 Preparation method of herbicide

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101935123A (en) * 2010-09-01 2011-01-05 合肥星宇化学有限责任公司 Method for recycling waste acid and waste residues in production of herbicide oxadiazon
CN105984916A (en) * 2015-02-10 2016-10-05 沈智奇 High-pressure, multiple-frequency and multiple-direction ultrasonic sewage purifier
CN109956537A (en) * 2019-03-26 2019-07-02 河北科技大学 A kind of processing method of the waste water containing acetone cyanohydrin
CN109956537B (en) * 2019-03-26 2021-10-15 河北科技大学 Treatment method of acetone-containing cyanohydrin wastewater
CN113003852A (en) * 2020-11-13 2021-06-22 四川全息生态环境技术产业有限公司 Ultrasonic wave and H2O2And micro-channel advanced oxidation method and device

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