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Polyimide/silica nanometer heavy metal adsorption material and its preparation and regeneration method

A technology of silica and polyimide, which is applied in chemical instruments and methods, separation methods, filter regeneration, etc., can solve problems such as poor recycling rate, non-hydrophilicity, and poor heat resistance, and achieve a solution Poor dispersibility, good hydrophilicity and dispersibility, good heat resistance

Active Publication Date: 2017-12-15
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The polymer adsorption materials currently used mainly include polyacrylamide, modified chitosan and modified cellulose, etc. Although these polymer adsorption materials have strong selectivity to heavy metal ions, due to their In terms of molecular main chain, they all belong to aliphatic polymer materials, so they generally have poor heat resistance. For example, the most commonly used polymer adsorption materials such as polyacrylamide are easy to degrade when used above 80°C for a long time, and the recycling rate is poor ( Kong Boling, Luo Jiuming.Research on the hydrolysis reaction of polyacrylamide under high temperature oil reservoir conditions[J].Petroleum Exploration and Development,1998,25(6):67-69.)
Although aromatic polyimide is a kind of organic polymer material with very good heat resistance, because the general polyimide structure does not contain groups that have complex adsorption for heavy metal ions, and it does not have affinity Water-based, so aromatic polyimide has almost no adsorption effect on heavy metal ions and cannot be used as an adsorption material

Method used

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  • Polyimide/silica nanometer heavy metal adsorption material and its preparation and regeneration method
  • Polyimide/silica nanometer heavy metal adsorption material and its preparation and regeneration method
  • Polyimide/silica nanometer heavy metal adsorption material and its preparation and regeneration method

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Embodiment 1

[0046] Under a nitrogen atmosphere, using PABZ and BPDA with a molar ratio of 1:1 as raw materials, first add the diamine monomer PABZ to N-methylpyrrolidone, stir at room temperature until it is uniformly dispersed, and then add the dianhydride monomer BPDA , continue to stir and react for 10 hours to obtain a BPDA / PABZ polyamic acid solution with a solid content of 10%, wherein the molar content of benzimidazole units is 50%; The base pyrrolidone was mixed according to the molar ratio of 1:4:1 and stirred at 40°C until the transparent sol of the silica precursor was obtained; The fraction is 10%, stirring and mixing evenly, and then stirring the mixed solution at 180° C. for co-heating precipitation reaction for 4 hours, filtering and drying.

[0047] The present invention has done following test investigation to present embodiment gained adsorption material:

[0048] 1) Dispersion status in water, see results figure 1 PI-10 in, and compared with the dispersion of the pol...

Embodiment 2

[0053] Under a nitrogen atmosphere, using PDA, PABZ and BPDA with a molar ratio of 5:5:10 as raw materials, first add the diamine monomers PDA and PABZ into N,N'-dimethylacetamide, and stir at room temperature Add the dianhydride monomer BPDA after it dissolves and disperses evenly, continue to stir and react for 8 hours to obtain a BPDA / PDA / PABZ polyamic acid solution with a solid content of 12%, wherein the molar content of the benzimidazole unit is 25%; Ethyl silicate, oxalic acid solution with pH=2 and N,N'-dimethylacetamide were mixed at a molar ratio of 1:4:1.5 and stirred at 50°C until a transparent sol of the silica precursor was obtained; BPDA / PDA / PABZ polyamic acid solution and the transparent sol of the silicon dioxide precursor are stirred and mixed uniformly according to the mass fraction of silicon dioxide being 50%, and then the mixed solution is stirred at 250° C. for co-thermal precipitation reaction for 3 hours, filtered, Just dry.

[0054] The adsorption c...

Embodiment 3

[0057] Under a nitrogen atmosphere, using ODA, PABZ and BPDA with a molar ratio of 3:7:10 as raw materials, first add the diamine monomers ODA and PABZ to N,N'-dimethylformamide, and stir at room temperature Add the dianhydride monomer BPDA after it dissolves and disperses evenly, continue to stir and react for 5 hours to obtain a BPDA / ODA / PABZ polyamic acid solution with a solid content of 15%, wherein the molar content of the benzimidazole unit is 35%; Ethyl silicate, nitric acid solution with pH=2 and N,N'-dimethylformamide were mixed at a molar ratio of 1:4:1.2 and stirred at 45°C until a transparent sol of the silica precursor was obtained; BPDA / ODA / PABZ polyamic acid solution and the transparent sol of the silicon dioxide precursor are stirred and mixed uniformly according to the mass fraction of the silicon dioxide being 30%, and then the mixed solution is stirred at 170° C. for co-thermal precipitation reaction for 3 hours, filtered, Just dry.

[0058] The adsorption...

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Abstract

The polyimide / silicon dioxide nanometer heavy metal adsorption material disclosed in the present invention is made by mixing the polyamic acid solution containing benzimidazole units and the silicon dioxide precursor sol evenly, and performing co-heat sinking at 150-250°C The adsorption material is a nanocomposite powder, the mass fraction of silicon dioxide contained in it is 5-50%, the mole fraction of benzimidazole units contained is 25-50%, and the first adsorption capacity is 20~80mg / g, the retention rate of adsorption capacity after 100 adsorption-regeneration cycles is ≥98%. The polyimide / silicon dioxide nanometer heavy metal adsorption material provided by the invention not only has good heat resistance, can be used for a long time in an environment below 250 ° C, and has a large amount of adsorption of heavy metal ions, and can also be used in the simple method provided by the invention With the matching of a reliable regeneration method, after 100 cycles of use, the retention rate of its adsorption capacity for heavy metals can remain above 98%, with long service life, low cost, more economical and environmentally friendly, and it also fills the gap in polymer high-temperature resistant adsorption materials .

Description

technical field [0001] The invention belongs to the technical field of heavy metal adsorption materials and their preparation and regeneration, and in particular relates to a polyimide / silicon dioxide nanometer heavy metal adsorption material and its preparation and regeneration methods. Background technique [0002] Heavy metals are a kind of accumulative and permanently harmful substances to the environment. As long as there are trace amounts in natural water bodies, they can produce toxic effects and cannot be converted into harmless substances through chemical or biological restoration processes. Their specific gravity is greater than 5g / cm 3 , there are about 45 kinds in nature, but in environmental science, people usually pay attention to several toxic heavy metals such as Hg, Cd, Pb, Cr, Cu, Co, Ni, etc. Organisms ingest heavy metals from the environment can be enriched tens of millions of times in higher organisms through the biomagnification of the food chain, and t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/26B01J20/30B01J20/34C02F1/28C02F101/20
Inventor 刘向阳罗龙波黄杰阳王旭李保印
Owner SICHUAN UNIV