Preparation method of silane modified attapulgite clay and application thereof in removing pesticide residues from Chinese herbal medicines

A silane modification, Chinese herbal medicine technology, applied in chemical instruments and methods, other chemical processes, ion exchange, etc., can solve the problems of complex methods and difficult to operate, and achieve the effects of abundant storage, easy access to prices, and no potential safety hazards.

Active Publication Date: 2018-12-25
HUAIYIN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The attapulgite prepared by silane modification reported in the literature is mostly used for wastewater treatment or metal ion adsorption, and it is relatively rare for the removal of pesticide residues in extracts of Chinese medicinal materials, and the method for preparing attapulgite by silane modification is also complicated and difficult to operate.

Method used

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  • Preparation method of silane modified attapulgite clay and application thereof in removing pesticide residues from Chinese herbal medicines
  • Preparation method of silane modified attapulgite clay and application thereof in removing pesticide residues from Chinese herbal medicines
  • Preparation method of silane modified attapulgite clay and application thereof in removing pesticide residues from Chinese herbal medicines

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Put the attapulgite and water in a beaker at a ratio of 1:20, stir at room temperature for 2 days, and let it stand for 2 days. After precipitation, take the middle layer and put it in another beaker. After replenishing water to the original volume, repeat the above steps 2-3 Second-rate. Finally, take the middle layer and place it in an oven at 105°C for drying, weighing, and grinding. Mix purified attapulgite with 1 mol·L -1 Acidify with hydrochloric acid at a ratio of 1:20, stir at room temperature for 2 days, let stand for 2 days, wash the clay solid in the lower layer with distilled water several times, filter with suction, dry, grind, pass through a 150-mesh sieve, and acidify the attapulgite. Take 10g of acidified attapulgite and 100mL of toluene in a 250mL three-necked flask, add 0.7g of KH-792, 1mL of triethylamine, stir magnetically, and heat to reflux for 24 hours. After the reaction, the attapulgite is washed repeatedly with ethanol until the coupling agent...

Embodiment 2

[0039] Put the attapulgite and water in a beaker at a ratio of 1:40, stir at room temperature for 2 days, and let it stand for 2 days. After precipitation, take the middle layer and put it in another beaker. After replenishing water to the original volume, repeat the above steps 2-3 Second-rate. Finally, take the middle layer and place it in an oven at 105°C for drying, weighing, and grinding. Mix purified attapulgite with 1 mol·L -1Acidify with hydrochloric acid at a ratio of 1:25, stir at room temperature for 2 days, let stand for 2 days, wash the lower clay solid with distilled water several times, filter with suction, dry, grind, pass through a 150-mesh sieve, and acidify the attapulgite. Take 10g of acidified attapulgite and 80mL of methanol-water into a 250mL three-necked flask, add 0.5g of KH-550 and 0.8mL of triethylamine, stir magnetically, and heat to reflux for 24 hours. After the reaction, attapulgite is washed repeatedly with ethanol until even The joint agent w...

Embodiment 3

[0042] Put the attapulgite and water in a beaker at a ratio of 1:50, stir at room temperature for 2 days, and let it stand for 2 days. After precipitation, take the middle layer and put it in another beaker. After replenishing water to the original volume, repeat the above steps 2-3 Second-rate. Finally, take the middle layer and place it in an oven at 105°C for drying, weighing, and grinding. Mix purified attapulgite with 1 mol·L -1 Acidify with hydrochloric acid at a ratio of 1:30, stir at room temperature for 2 days, let stand for 2 days, wash the clay solid in the lower layer with distilled water several times, filter with suction, dry, grind, pass through a 150-mesh sieve, and acidify the attapulgite. Take 10g of acidified attapulgite and 120mL of ethanol-water into a 250mL three-necked flask, add 1g of KH-1161 and 1.2mL of triethylamine, stir magnetically, and heat to reflux for 24 hours. After the reaction, the attapulgite is washed repeatedly with ethanol until coupli...

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Abstract

The invention discloses a preparation method of silane modified attapulgite clay and application thereof in removing pesticide residues from Chinese herbal medicines. The preparation method of the silane modified attapulgite clay includes purification of attapulgite, acidification and silane modification of the attapulgite clay. The application steps of the silane modified attapulgite clay in removing the pesticide residues from Chinese herbal medicines include weighing Chinese herbal medicine extracts, and placing the silane modified attapulgite clay in a mixed pesticide aqueous solution; performing shock adsorption at the constant temperature of 15-25 DEG C for 1-2 hours; centrifuging with the rotating speed of 11000 r / min<-1> for 5-10 minutes; adopting GC-MS / MS to analyze the pesticidecontent of supernatant liquid; and adopting the GC-MS / MS to analyze the pesticide content of raw materials in the traditional Chinese medicine extracts. The method of the invention has the advantagesof simple process, convenient operation and no potential safety hazard; the pesticide residues in the traditional Chinese medicine extracts meet the maximum pesticide residue limit standards of countries and regions such as China, the European Union, the United States and the like after being removed; and moreover, the attapulgite clay is abundant in storage and low in price in China.

Description

technical field [0001] The invention belongs to the technical field of natural mineral utilization, and relates to a preparation method and application of modified attapulgite, in particular to a preparation method of silane-modified attapulgite and its application in the removal of pesticide residues in Chinese herbal medicines. Background technique [0002] With the advent of the "big health era", traditional Chinese medicine in our country plays an irreplaceable role and is widely used in the development of drugs and functional foods. [0003] In the process of planting Chinese medicinal materials, in order to prevent losses caused by pests and diseases, pesticide farmers inevitably use pesticides to reduce risks. Therefore, excessive pesticide residues seriously lag behind the pace of innovation and development of Chinese medicinal materials in my country. At present, the residual pesticides in traditional Chinese medicinal materials are mainly organochlorines, organopho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/12B01J20/30B01D15/08
CPCB01D15/08B01J20/12
Inventor 喻春皓王亚茹邹雯燕夏尧干冒顾政宋悉玲周跃刘雨婷胡天乐焦晓薇刘彤
Owner HUAIYIN INSTITUTE OF TECHNOLOGY
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