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Magnetic sulphonated carbon-based nanofiber, preparation method for same and application thereof

A technology for sulfonating carbonyl nanometer and carbon-based fibers, which is applied in chemical instruments and methods, fiber chemical characteristics, spinning solution preparation, etc., can solve the problems of excessive waste liquid, high preparation cost, poor stability, etc., and achieve simple process, The effect of wide range of raw materials and low price

Active Publication Date: 2012-06-20
JIANGSU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The solid acid catalyzed transesterification process not only avoids serious problems such as difficult catalyst separation, excessive waste liquid, and strong corrosion in the reaction, but also has the advantages of mild reaction conditions, reusable catalysts, easy automatic continuous production, and no pollution to the environment. At present, the commonly used solid acid catalysts in the preparation of biodiesel include: zeolite molecular sieves, heteropolyacids, ion exchange resins and solid superacids, etc., but these solid acid catalysts have high preparation costs, low catalytic activity, and stability during use. It is difficult to realize industrial application due to a series of problems such as poor performance and poor reusability. Therefore, the research and development of cheap, efficient and stable solid acid catalysts is very important for the development of biodiesel industry.

Method used

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  • Magnetic sulphonated carbon-based nanofiber, preparation method for same and application thereof
  • Magnetic sulphonated carbon-based nanofiber, preparation method for same and application thereof
  • Magnetic sulphonated carbon-based nanofiber, preparation method for same and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1 (magnetic sulfonated carbon-based fiber):

[0031] Step 1: get 8g ferric nitrate (Fe(NO 3 ) 3 9H 2 O), 9g glucose (D-(+)-Glucose), mixed in 400ml deionized water, Fe 3+ The molar concentration of G is 0.0495mol / L, and the molar concentration of G is 0.1135mol / L The raw material mass ratio is: Fe 3+ :G=8:9, then perform magnetic stirring for 24 hours.

[0032] Step 2: Then put the precursor solution into a vacuum rotary evaporator, depressurize at 70°C, and dehydrate it for 45 minutes at a pressure of 0.05Mpa to obtain a gel colloid.

[0033] Step 3: Put the gel obtained in step 2 into an oven, dry and dehydrate at 60°C, place it in the oven for 1 hour, then pull the gel into gel cellulose filaments, place the cellulose filaments Dry in a crucible at 100°C.

[0034] Step 4: The fiber precursor is heated up to 400°C at a heating rate of 3°C / min in an air atmosphere, and kept for 5 hours; naturally cooled to obtain the target carrier Fe / C fiber with a di...

Embodiment 2

[0037] Example 2 (magnetic sulfonated carbon-based fibers):

[0038] Step 1: get 14g ferric nitrate (Fe(NO 3 ) 3 9H 2 O), 18g glucose solid powder (D-(+)-Glucose), mixed in 500ml deionized water, Fe 3+ The molar concentration of G is 0.0693mol / L, the molar concentration of G is 0.1818mol / L, and the mass ratio of raw materials is: Fe 3+ :G=7:8, then perform magnetic stirring for 24 hours.

[0039] Step 2: Then put the precursor solution into a vacuum rotary evaporator, depressurize at 63°C, dehydrate at 0 MPa, and dehydrate for 60 minutes to obtain a gel colloid.

[0040] Step 3: The gel obtained in step 2 was spun on a self-made gel spinning machine, and the collected cellulose filaments were dried in an oven at 90°C.

[0041] Step 4: Heat the fiber precursor to 350°C at a heating rate of 3°C / min in an air atmosphere, and keep it for 8 hours; cool naturally to obtain the target carrier Fe / C-SO with a diameter of micron 3 H fiber.

[0042] Step 5: Immerse 2 g of the c...

Embodiment 3

[0044] Example 3 (magnetic sulfonated carbon-based fibers):

[0045] Step 1: get 12g ferric nitrate (Fe(NO 3 ) 3 9H 2 O), 14g glucose solid powder (D-(+)-Glucose), mixed in 500ml deionized water, Fe 3+ The molar concentration of G is 0.0594mol / L, and the molar concentration of G is 0.1413mol / L The raw material mass ratio is: Fe 3+ :G=6:7, then perform magnetic stirring for 24 hours.

[0046] Step 2: Then put the precursor solution into a vacuum rotary evaporator, depressurize at 63°C, the pressure is about 0Mpa, and dehydrate for 70 minutes to obtain a gel colloid.

[0047] Step 3: The gel obtained in step 2 is spun on a gel spinning machine, and the collected cellulose filaments are dried in an oven at 90°C.

[0048] Step 4: Heat the fiber precursor to 380°C at a heating rate of 3°C / min in an air atmosphere, and keep it warm for 6 hours; naturally cool to obtain the target carrier Fe / C-SO with a diameter of micron 3 H fiber.

[0049] Step 5: Immerse 2 g of the carri...

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Abstract

The invention relates to the field of inorganic nonmetal materials, in particular to a magnetic sulphonated carbon-based nanofiber, a preparation method for same and application thereof. Glucose and ferric nitrate are proportionally mixed and dissolved and chemically react to prepare precursor sol, the precursor sol is subjected to decompression dehydration to obtain precursor gel with certain viscosity, the precursor gel is spun into gel cellulose fibers, the obtained gel cellulose fibers are incompletely carbonized at 350-400 DEG C in the presence of N2, and then 95% concentrated sulfuric acid 200ml is added to the carbonized gel cellulose fibers for sulphonating at 80-100 DEG C for 8 hours. Initially, the magnetic sulphonated carbon-based nanofiber with uniform diameter, large specific surface area, larger length-diameter ratio and high magnetism is prepared from the glucose and the ferric salt by means of organic gel precursor conversion and under actions of incomplete carbonization and sulphonation, and is highly active when used for catalyzing conversion of high-acid grease into biodiesel. Recycling the nanofiber is possible due to a certain magnetism of the nanofiber.

Description

technical field [0001] The invention relates to the field of inorganic non-metallic materials, in particular to a magnetic sulfonated carbon-based nano hollow fiber and its preparation method and application. Background technique [0002] With the depletion of petroleum resources, the supply of petrochemical diesel is becoming increasingly tight. Biodiesel is expected to replace petrochemical diesel fuel and meet people's needs because of its environmental friendliness and renewable. Various oils and methanol or ethanol are used as raw materials, and are obtained through transesterification reactions with acids, alkalis, enzymes, etc. as catalysts or under supercritical conditions. [0003] Generally, basic catalysts such as sodium hydroxide and potassium hydroxide are mostly used in industrial biodiesel production, but the use of basic catalysts has very strict requirements on raw oils and fats. Not more than 0.1-0.3% (moisture in raw materials will promote the hydrolysis ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/10D01F11/00D01D1/02D01D5/04B01J27/02C11C3/10C10L1/02
CPCY02E50/13Y02E50/10
Inventor 林琳崔凤杰武文钰孙文敬周强
Owner JIANGSU UNIV
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