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Method for removing trace diquat in water

A diquat and trace technology, which is applied in separation methods, chemical instruments and methods, water pollutants, etc., can solve the problems of small volume of water samples, high cost of solid-phase extraction cartridges, and difficulty in popularization, etc., so as to save consumption, Remarkable processing effect, convenient and quick operation

Active Publication Date: 2020-06-12
ZHEJIANG GONGSHANG UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The adsorption of diquat in water mainly adopts weak cation exchange WCX cartridges and solid phase extraction method (Wang Jing, Liu Zhengzheng. Solid phase extraction-liquid chromatography / ultraviolet method for the determination of paraquat and diquat in surface water. China Environmental Monitoring, 2011,27(4):50-51; Chen Jing, Liu Zhaojin, An Baochao, Lu Yan, Xu Qun. Determination of paraquat and diquat in drinking water and environmental water by on-line purification / solid phase extraction-high performance liquid chromatography Fast, Chromatography, 2012, 30(10):1068-1073) for adsorption, can better enrich diquat in water, but the cost of WCX solid-phase extraction column is high, the volume of purified water sample is small, and it is not easy to treat in water Effective promotion in practical application

Method used

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  • Method for removing trace diquat in water
  • Method for removing trace diquat in water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] In a 200mL beaker, add 1.0g of Fe(NO 3 ) 3 ·9H 2 O, 1.0g of Mn(NO 3 ) 2 ·4H 2 O and 1.0g of ZrCl 4 After mixing, add 5.0mL of 0.1mol / L hydrochloric acid and 80mL of DMF and stir to dissolve. After the dissolution is complete, add 2.0g of 2-aminoterephthalic acid, stir and mix, and transfer to a 250mL pressure-resistant closed reactor after dissolution. After cooling, the reaction solution was transferred to a 100mL centrifuge tube and centrifuged at 3000rpm to obtain a crude product. The product was washed twice with 20mL DMF and 20mL ethanol, and then the product powder was placed Put it in a 50mL colorimetric tube with a stopper, soak in absolute ethanol for 72 hours, and finally vacuum dry at room temperature to obtain Fe / Zr / Mn-MOFs. The SEM image is shown in figure 1 , The particle size is about 100-300μm.

[0035] The prepared Fe / Zr / Mn-MOFs material is mixed with quartz sand with a particle size of 0.05mm~0.1mm in a weight ratio of 2:1 and then uniformly filled in the ...

Embodiment 2

[0037] In a 200mL beaker, add 1.0g of Fe(NO 3 ) 3 ·9H 2 O, 2.0g of Mn(NO 3 ) 2 ·4H 2 O and 1.5g of ZrCl 4 After mixing, add 5.0mL of 0.1mol / L hydrochloric acid and 80mL of DMF and stir to dissolve. After the dissolution is complete, add 2.5g of 2-aminoterephthalic acid, stir and mix, and then transfer to 250mL pressure-resistant airtight reaction after dissolution In the kettle, react at 90°C for 15 hours. After cooling, transfer the reaction solution to a 100 mL centrifuge tube and centrifuge at 3000 rpm to obtain a crude product. Wash the product twice with 20 mL DMF and 20 mL ethanol. The 50mL colorimetric tube of the stopper was soaked in absolute ethanol for 72 hours, and finally dried under vacuum at room temperature to obtain Fe / Zr / Mn-MOFs material with a particle size of about 100-300 μm.

[0038] The Fe / Zr / Mn-MOFs material obtained is mixed with quartz sand with a particle size of 0.1mm~0.5mm at a weight ratio of 3:1 and then uniformly filled in the chromatography filter ...

Embodiment 3

[0040] In a 200mL beaker, add 1.0g of Fe(NO 3 ) 3 ·9H 2 O, 2.5g of Mn(NO 3 ) 2 ·4H 2 O and 0.5g of ZrCl 4 After mixing, add 5.0mL of 0.1mol / L hydrochloric acid and 80mL of DMF and stir to dissolve. After the dissolution is complete, add 1.5g of 2-aminoterephthalic acid, stir and mix, and then transfer to 250mL pressure-resistant airtight reaction In the kettle, react at 100°C for 18 hours. After cooling, transfer the reaction solution to a 100mL centrifuge tube, centrifuge at 3000rpm to obtain a crude product, and rinse it with 20mL DMF and 20mL ethanol twice. The product powder is placed in A 50mL colorimetric tube with a stopper was soaked in absolute ethanol for 72 hours, and finally dried in a vacuum at room temperature to obtain Fe / Zr / Mn-MOFs with a particle size of about 100-300 μm.

[0041] Mix the obtained Fe / Zr / Mn-MOFs material with quartz sand with a particle size of 0.1mm~0.5mm at a weight ratio of 4:1 and evenly fill it in the chromatography filter column. At the same ...

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Abstract

The invention discloses a method for removing trace diquat in water. The method comprises the following steps: (1) uniformly mixing Fe(NO3)<3>.9H2O, Mn(NO3)<2>.4H2O and ZrCl4 according to a certain weight ratio and then dissolving the mixture into hydrochloric acid; adding DMF, then adding 2-aminoterephthalic acid; dissolving, transferring the obtained solution into a closed reaction container, reacting at 80-120 DEG C for 10-30 hours, carrying out centrifugal separation to obtain a crude product, washing the crude product with DMF and ethanol in sequence, soaking product powder into absoluteethyl alcohol for 72 hours, and finally, carrying out vacuum drying at room temperature to obtain a Fe / Zr / Mn-MOFs material; 2) mixing the prepared Fe / Zr / Mn-MOFs material with quartz sand according toa weight ratio of (1-5):1, and uniformly filling a chromatographic filter column with the obtained mixture so as to obtain a chromatographic filter column filled with the Fe / Zr / Mn-MOFs-quartz sand adsorption material; and 3) pumping micro-polluted water containing diquat from the bottom end of the chromatographic filter column obtained in the step 2), and enabling the micro-polluted water to passthrough the chromatographic filter column at a flow rate of 1-30 mL / min and flow out from the top end of the column. The method is simple in process, convenient and quick to operate, remarkable in treatment effect and suitable for removing diquat in micro-polluted water.

Description

Technical field [0001] The invention belongs to the technical field of water purification treatment, and specifically relates to a method for removing trace diquat in water. Background technique [0002] Diquat dibromide (CAS:85-00-7) is a broad-spectrum herbicide of quaternary ammonium salt, which is widely used in the control of aquatic weeds. It also has a strong ability to control broad-leaved weeds. It can also be used as a desiccant for seed plants, an inactivator for soybeans, corn, rice, etc., and an inhibitor for sugarcane inflorescence. According to my country's pesticide toxicity classification standards, Diquat is moderately toxic, has moderate irritation to eyes and skin, is toxic to mammals, and can cause fetal malformations. With the increasing production and usage of Diquat, it has become one of the important pollution sources of drinking water. [0003] The adsorption of diquat in water mainly uses weak cation exchange WCX cartridges and solid phase extraction (W...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01D15/22C02F1/28B01J20/30C02F101/30
CPCB01D15/22B01J20/16B01J20/226C02F1/281C02F1/285C02F2101/306
Inventor 蔡美强金米聪宋志军徐晓杰连广浒沈鑫杰毛佳琪魏宗苏施跃锦温玉婷
Owner ZHEJIANG GONGSHANG UNIVERSITY
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