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Preparation method of graphene/polyimide composite sponge with multilevel structure

A technology of polyimide and composite sponge, which is applied in the field of adsorption materials, can solve the problems of heavy metal ions, organic solvents and dyes, single adsorption structure of materials, and high preparation cost, so as to improve hydrophobic/lipophilic properties and simplify the processing flow , Improve the effect of adsorption effect

Pending Publication Date: 2022-04-26
NORTHWEST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

A large number of results show that the mechanical properties such as glass transition temperature, thermal stability, Young's modulus and elongation strength of the graphene sponge after polymer modification are significantly improved, but there is still a single material adsorption structure and relatively low preparation cost. In addition, the current graphene sponge mainly realizes the adsorption of pollutants through the three-dimensional graphene network structure, and its cavity pore size and porosity are relatively fixed.
In the actual pollution treatment, the diameter of petroleum pollutants in oily wastewater is between 20 and 100 μm. In addition to the sudden crude oil leakage accompanying the chemical production process and the non-point source pollution in the mining area, the wastewater contains petroleum organic matter. , may also contain many other pollutants such as heavy metal ions, organic solvents and dyes, so it is difficult for a graphene sponge with a fixed pore size to simultaneously adsorb various pollutants of different sizes

Method used

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  • Preparation method of graphene/polyimide composite sponge with multilevel structure
  • Preparation method of graphene/polyimide composite sponge with multilevel structure
  • Preparation method of graphene/polyimide composite sponge with multilevel structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1. Disperse 60mg of graphene evenly in 10mL of deionized water, then add 0.6g of polyethylene glycol and stir for 2 hours, and perform dialysis with a dialysis bag with a molecular weight cut-off of 6000Da to remove ungrafted polyethylene glycol, and obtain the mass The volume concentration is 6mg / mL graphene dispersion.

[0028] 2. Weigh 0.04g of silicon dioxide and add it into 1mL N,N-dimethylformamide and stir evenly, then slowly add 0.008g of 3-glycidyloxypropyltrimethoxysilane, stir at 40°C for 30 Minutes, then add 0.07g 4,4'-diaminodiphenyl ether under ice bath conditions, mechanically stir with nitrogen, add 0.08g pyromellitic anhydride in batches, stir and react at room temperature for 3 hours, then add 0.05g Tris Ethylamine, after stirring evenly, the resulting solution was dissolved in 20 mL of deionized water to obtain a golden yellow polyamic acid solution A1 containing silicon dioxide.

[0029] 3. Mix the polyamic acid solution A1 obtained in step 2 with t...

Embodiment 2

[0036] 1. Disperse 60mg of graphene evenly in 10mL of deionized water, then add 0.6g of polyethylene glycol and stir for 2 hours, and perform dialysis with a dialysis bag with a molecular weight cut-off of 6000Da to remove ungrafted polyethylene glycol, and obtain the mass The volume concentration is 6mg / mL graphene dispersion.

[0037] 2. Add 0.07g of 4,4'-diaminodiphenyl ether into 1mL of N,N-dimethylformamide under ice bath conditions, mechanically stir with nitrogen gas, and add 0.08g of pyromellitic anhydride in batches Finally, stir for 30 minutes, then add 0.05g polyetheramine, stir and react at room temperature for 3 hours, then add 0.05g triethylamine, stir evenly and dissolve the resulting solution in 20mL deionized water to obtain polyamic acid containing polyetheramine Solution C1.

[0038] 3. Mix the polyamic acid solution C1 obtained in step 2 with the graphene dispersion obtained in step 1 evenly, stir at room temperature for 1 hour, so that the polyamic acid i...

Embodiment 3

[0043] 1. Disperse 60mg of graphene evenly in 10mL of deionized water, then add 0.6g of polyethylene glycol and stir for 2 hours, and perform dialysis with a dialysis bag with a molecular weight cut-off of 6000Da to remove ungrafted polyethylene glycol, and obtain the mass The volume concentration is 6mg / mL graphene dispersion.

[0044] 2. Add 0.07g of 4,4'-diaminodiphenyl ether into 1mL of N,N-dimethylformamide under ice bath conditions, mechanically stir with nitrogen gas, and add 0.08g of pyromellitic anhydride in batches Finally, stir and react at room temperature for 3 hours, then add 0.05g of triethylamine, stir evenly, dissolve the resulting solution in 20mL of deionized water, add 0.05g of paraffin and 0.05g of dodecylphenol polyoxyethylene ether, and use emulsifying shears Switch to a stirrer and stir evenly to obtain polyamic acid solution B1 containing paraffin wax and dodecylphenol polyoxyethylene ether.

[0045] 3. Add the graphene dispersion obtained in step 1 t...

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Abstract

The invention discloses a preparation method of graphene / polyimide composite sponge with a multilevel structure, which comprises the following steps: firstly, hydroxylating graphene by using polyethylene glycol to improve the grafting rate of a polymer chain on the surface of the graphene; the preparation method comprises the following steps: preparing graphene, grafting a polyimide chain on the surface of a graphene sheet layer by utilizing an esterification reaction of a large amount of active hydroxyl on the surface of the graphene and a polyimide chain terminal anhydride group, and introducing a removable pore-foaming agent on the polyimide chain to form nanopores. In the thermal reduction process, the structure and morphology of the graphene / polyimide composite sponge on a graphene sheet layer can be stably maintained, and finally the three-dimensional graphene / polyimide multilevel structure composite sponge with macroporous graphene as a framework and a polyimide chain as a modification is formed. The specific surface area of the composite sponge can be greatly increased through construction of the multi-stage structure, various pollutants with different molecular sizes can be adsorbed at the same time through holes and material gaps with different pore diameters in the composite sponge, the adsorption efficiency of the composite sponge is improved, and the oil pollution treatment process is simplified.

Description

technical field [0001] The invention belongs to the technical field of adsorption materials, and in particular relates to a preparation method of a multi-level structure graphene / polyimide composite sponge. Background technique [0002] In recent years, the occurrence of sea oil spills, the oily wastewater produced by humans and the use of organic solvents have caused serious harm to water resources. Due to the advantages of low cost and environmental friendliness, physical adsorption has become the most commonly used method to treat water pollution. However, the adsorption capacity of traditional oil-absorbing materials needs to be improved, so it is urgent to develop high-performance adsorption materials. Graphene sponge is a three-dimensional mesh porous material with high adsorption capacity for oil pollution. However, it is difficult for current graphene sponge to have strong mechanical properties and thermal stability, which is not conducive to the reuse of materials. ...

Claims

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Application Information

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IPC IPC(8): C08L79/08C08K9/04C08K3/04C08J9/26C08G73/10
CPCC08J9/26C08J9/009C08G73/1071C08J2379/08C08J2201/044
Inventor 鲍琳鱼萍张镇宇秦晶晶黄可欣
Owner NORTHWEST UNIV