Preparation method and application of organic isocyanate-and-isorhodanate modified attapulgite

A technology for modifying attapulgite and isothiocyanate, which is applied in chemical instruments and methods, silicate, aluminum silicate, etc., can solve the problems of restricting the application of attapulgite, and achieve a simple preparation method, which is beneficial to The effect of popularization and use and low preparation cost

Active Publication Date: 2017-04-12
HUAIYIN TEACHERS COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the special structure of attapulgite also causes the surface of attapulgite to be often covered with water film, which limits the application of attapulgite in some fields

Method used

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  • Preparation method and application of organic isocyanate-and-isorhodanate modified attapulgite
  • Preparation method and application of organic isocyanate-and-isorhodanate modified attapulgite
  • Preparation method and application of organic isocyanate-and-isorhodanate modified attapulgite

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Experimental program
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preparation example Construction

[0025] The embodiment of the present invention provides a method for preparing organic isocyanate and isothiocyanate modified attapulgite, comprising the following steps:

[0026] S1. Add attapulgite raw soil through a 100-300 mesh sieve into the reactor, and add 3-4mol / L of HCl or HNO 3 After soaking 20-50mL for 24h, wash with deionized water until neutral, and dry at 105°C-120°C.

[0027] S2. Weigh 200 mg of the pretreated and dried attapulgite obtained in step S1 and place it in an ethanol solution, and add about 0.45 mmol-1.0 mmol of 3-aminopropyltrimethoxysilane. Stir for 3-6h in the temperature range of -8°C-40°C. Filter and wash, and dry at 105°C-120°C.

[0028] S3. Add 0.46-1 mmol isocyanate and isothiocyanate ethanol solution to the ethanol solution of attapulgite obtained in step S2, reflux and stir at a temperature of about 80°C for 1-5h, filter, wash, and vacuum dry at about 85°C Obtain organic isocyanate and isothiocyanate modified attapulgite.

[0029] In ste...

Embodiment 1

[0043] (1) Pretreatment of attapulgite. Add 5g of attapulgite raw soil passed through a 200-mesh sieve into the reactor, add 30mL of 3-4mol / L HCl, soak for 24h, wash with deionized water until neutral, and dry at 105°C.

[0044] (2) Weigh 200 mg of pretreated and dried attapulgite and place it in 20 mL of ethanol solution, and add about 0.45 mmol of 3-aminopropyltrimethoxysilane. Stir internally for 4 h at a temperature of 10 °C. Filter washed and dried at 105°C.

[0045] (3) Add 0.45-1 mmol ethanol solution of p-nitrophenylisocyanate to 200 mg of the product obtained in (2), and reflux and stir at about 80° C. for 2 h. Filtrate, wash, and vacuum-dry at about 85°C to obtain p-nitrophenylisocyanate-modified attapulgite.

[0046] (4) Determine the chromatographic working conditions. Select chromatographic column: Inertisil-ODS-SP C18, 4.6×150mm, 5 μm, mobile phase is acetonitrile:water=20:80 (V / V), flow rate 1.00mL min -1 , column temperature 25°C, UV detection wavelength: ...

Embodiment 2

[0052] (1) Pretreatment of attapulgite. Add 5g of attapulgite raw soil through a 200-mesh sieve into the reactor, add 3-4mol / L of HNO 3 After soaking 30mL for 24h, wash with deionized water until neutral, and dry at 105°C.

[0053] (2) Weigh 200 mg of pretreated and dried attapulgite into 20 mL of ethanol solution, and add about 0.6 mmol of 3-aminopropyltrimethoxysilane. Stir internally at 10 °C for 3 h. Filter washed and dried at 105°C.

[0054] (3) Add 1 mmol ethanol solution of p-toluene isocyanate to 200 mg of the product obtained in (2), and stir under reflux at a temperature of about 80° C. for 2 h. Filtrate, wash, and vacuum-dry at about 85°C to obtain p-toluene isocyanate-modified attapulgite.

[0055] (4) Determine the chromatographic working conditions. Select chromatographic column: Inertisil-ODS-SP C18, 4.6×150mm, 5 μm, mobile phase is acetonitrile:water=20:80 (V / V), flow rate 1.00mL min -1 , column temperature 25°C, UV detection wavelength: 254nm, injection ...

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Abstract

The invention discloses a preparation method and application of organic isocyanate-and-isorhodanate modified attapulgite. The preparation method comprises the following steps: introducing amino groups onto raw attapulgite by using a simple stirring method; and then carrying out reflux in an ethanol solution in virtue of the chemical combination action of the amino groups with isocyanate and isorhodanate so as to obtain the organic isocyanate-and-isorhodanate modified attapulgite. With the modified attapulgite as an adsorbent and pesticides and herbicides like pymetrozine, thiamethoxam, weeding bensulfuron methyl and the like as adsorption objects, studies are carried out on the removal effect of the adsorbent on dense residual pesticides and herbicides in water. Experimental results show that the modified attapulgite exerts excellent adsorption and removal effect on pymetrozine, thiamethoxam, bensulfuron methyl and the like. Application of the modified attapulgite has the advantages of low price, simple preparation, high adsorption efficiency and the like; and the modified attapulgite has practical value in rapid removal of dense residual pesticides and herbicides in water bodies.

Description

technical field [0001] The invention relates to the field of material preparation, in particular to a preparation method and application of organic isocyanate and isothiocyanate modified attapulgite. Background technique [0002] Pesticides and herbicides are widely used in our country. In view of the general toxicity of pesticides and herbicides, it is inevitable to have direct or indirect effects on humans. For example, thiamethoxam can induce liver tumors in mice; pymetrozine can cause tumors in mice; bensulfuron-methyl has genotoxic effects on zebrafish, and can induce a significant increase in the rate of micronuclei in red blood cells. It has been reported that amide herbicides (bensulfuron-methyl belongs to this category of substances) can be degraded and converted into carcinogenic dialkylquinone imines. Therefore, all countries in the world have made specific regulations on the residues of pesticides and herbicides in crops. In recent years, all river basins in m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/16B01J20/30C02F1/28
Inventor 张宇赵剑英夏敏唐果东鲁媛魏文华鲍倩马莤莤
Owner HUAIYIN TEACHERS COLLEGE
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