Magnetic separation type composite adsorbing material and preparation method thereof

A composite adsorption material, magnetic separation technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problem of reaction mechanism analysis, solvent recovery and waste liquid treatment difficulties, unable to meet actual production and large-scale applications, solvents and various Auxiliaries are not common in price and other problems, and achieve the effects of good external magnetic field reaction ability, lower synthesis cost, and simple and easy preparation method.

Inactive Publication Date: 2011-01-12
FUZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, in recent years, the synthesis of nano-Fe by low-temperature solvothermal reaction 3 o 4 Materials are favored. For example, Yasuhiro et al. synthesized 100 nm highly crystalline monodisperse Fe by pyrolysis and reduction of Fe(Ⅲ) C10 tertiary carbonic acid complex salt in C10 tertiary carbonic acid. 3 o 4 Nanocrystals; Pinna group and Kominami group used Fe(acac)3 in benzyl alcohol and propanol solutions to obtain Fe(acac)3 solvothermally with a size of 10 nm 3 o 4 Nanoparticles, in practical applications such as catalysis, these nanoparticles still need to be loaded on some kind of substrate. For this reason, they are often firmly attached by sintering and other methods, but these processes often have negative effects such as reduction of active sites and particle agglomeration. effect
If Fe 3 o 4 One-time synthesis on the surface of the carrier can overcome the above shortcomings, but the Fe 3 o 4 There are few reports on the loading of nanomaterials
In addition, because the existing solvothermal synthesis system of iron oxides puts too much emphasis on its controllability, the design of the system is relatively complicated, resulting in a wide variety of transition species and by-products in the system. etc. have brought many difficulties, and the solvents and various additives used are uncommon and expensive, which cannot meet the needs of actual production and large-scale applications.

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  • Magnetic separation type composite adsorbing material and preparation method thereof
  • Magnetic separation type composite adsorbing material and preparation method thereof
  • Magnetic separation type composite adsorbing material and preparation method thereof

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preparation example Construction

[0027] The preparation steps of the present invention are as follows:

[0028] 1. Activated carbon fiber pretreatment

[0029] Activated carbon fiber (ACF) is a PAN (polyacrylonitrile)-based, 1.5mm thick industrial activated carbon fiber felt product purchased directly, with a specific surface area of ​​1402m 2 / g. First cut the carbon felt into small pieces of 5×15 cm, then impregnate it with a certain volume of 67% concentrated nitric acid (according to the submerged ACF), seal it and let it stand for more than 12 hours, take it out and rinse it with deionized water until the pH value is 6.5, Dry it thoroughly in an oven at 150°C, and store it in an oven at 120°C for future use.

[0030] 2. Nano Fe 3 o 4 One-step solvothermal synthesis of composites with ACF fibers

[0031] Accurately weigh 1.25g Fe(acac)3 (iron acetylacetonate) into a 150ml thoroughly dried Erlenmeyer flask with a stopper, accurately measure 70ml of organic solvent with a measuring cylinder, add it in...

Embodiment 1

[0034] (1) Preparation of nano Fe3O4 and ACF composite fiber adsorption material by solvothermal in situ reduction reaction with ethanol as solvent

[0035] The synthesis steps are equivalent to the preparation steps in the specific embodiments of the invention above, using ethanol as the organic solvent, and the reaction temperatures are 160°C and 190°C respectively. Such as figure 1 According to the XRD spectrum, the composition of oxides in the products synthesized at two temperatures is Fe3O4, and the crystal phase is perfect. However, it can be seen from the XRD spectrum that the product loading at 160°C is much less than that of the sample at 190°C. The particle sizes of the oxide crystal phase in FE-18-160 (composite sample obtained after 18h reaction at 160°C) and FE-18-190 (composite sample obtained after 190°C reaction for 18h) were estimated to be 18.2 nm and 17.1 nm, respectively nm. FESEM image of FE-18-160 ( figure 2 ) in the distribution of the oxide partic...

Embodiment 2

[0044] The concrete steps of the preparation method of a kind of magnetic separation type composite adsorption material are:

[0045] 1) Activated carbon fiber pretreatment

[0046] Impregnate the activated carbon fiber ACF with 75% concentrated nitric acid, subject to the immersion of the ACF, seal it and let it stand for 48 hours, take it out and rinse it with deionized water until the pH value is 6, then dry it thoroughly in an oven at 100°C, and put it in an oven at 120°C Save for later.

[0047] 2) Nano Fe 3 o 4 One-step solvothermal synthesis of composites with ACF fibers

[0048] Accurately weigh 4g of iron acetylacetonate and put it into a 500mL thoroughly dried Erlenmeyer flask with a stopper, add 150ml of acetone to it with a measuring cylinder, seal it, and ultrasonically disperse it for 45 minutes to obtain nano-Fe 3 o 4 . Take 2g of ACF treated in step 1) and immerse in the prepared solution, seal it, and ultrasonically degas it for 120 minutes, then mov...

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Abstract

The invention relates to a magnetic separation type composite adsorbing material which is prepared from nano Fe3O4 and active carbon fiber. The ferriferous oxide nano composition fiber material is synthesized by using conventional organic solvent as the reaction medium under the control of a simple low temperature solvent thermal system. The magnetic separation type composite adsorbing material can be used as a magnetic separation type adsorbing material for adsorbing organic or inorganic pollutants to purify waste water.

Description

technical field [0001] The invention belongs to the field of composite materials, and more specifically relates to a magnetic separation type composite adsorption material and a preparation method thereof. Background technique [0002] Iron oxide is a very common catalyst or carrier. It is also commonly used in the removal and recovery of various inorganic and organic pollutants in water. It is also the most widely studied sensor material, such as humidity-sensitive, temperature-sensitive, and gas-sensitive materials. Its microwave and The optical absorption effect is also very good. Fe in iron oxide 3 o 4 It is a ferrite material with a typical inverse spinel structure, showing special electrical, magnetic, catalytic and other properties. And Fe 3 o 4 Good compatibility with the environment and organisms, these advantages prompt people to try to compound it with other inorganic, organic or biological materials to obtain multi-component catalysts or carriers, magnetica...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/20B01J20/30
Inventor 员汝胜付贤智王占义刘平陈旬李朝晖王绪绪吴棱戴文新
Owner FUZHOU UNIV
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