Method for preparing lignin-based carbon fiber hydrogen storage material by electrostatic spinning process

An electrospinning, lignin-based technology, applied in fiber processing, fiber chemical characteristics, filament/thread forming, etc., can solve the problems of limited reserves, high price, environmental pollution, etc., and achieve easy operation, low price, The effect of high degree of graphitization

Active Publication Date: 2015-09-30
QUANGANG PETROCHEM RES INST OF FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, more than 90% of carbon fibers currently on the market are made of polyacrylonitrile, which is a petroleum-based raw material, not only has limited reserves, is expensive, and the exploitation of petrochemical resources will also cause a certain degree of pollution to the environment

Method used

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  • Method for preparing lignin-based carbon fiber hydrogen storage material by electrostatic spinning process
  • Method for preparing lignin-based carbon fiber hydrogen storage material by electrostatic spinning process
  • Method for preparing lignin-based carbon fiber hydrogen storage material by electrostatic spinning process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1. Preparation of spinning solution: Take 1 g of LN, 1 g of PAN, 0.4 g of nickel acetate, 0.1 g of boric acid and 17 ml of DMF, and stir on a magnetic stirrer at 25 °C until completely dissolved to form a uniform spinning solution .

[0028] 2. Preparation of composite fibers by electrospinning: Under the conditions of voltage 18 kv, receiving distance 15 cm, spinning solution flow rate 0.8 ml / h, and electrospinning temperature 45 ℃, LN / PAN composite micro-nano fibers were obtained by electrospinning and dried in a vacuum oven at 70 °C for 8 h.

[0029] 3. Pre-oxidation: The dried LN / PAN composite micro-nanofibers were pre-oxidized at 280 °C for 1 h in an air atmosphere in a muffle furnace.

[0030] 4. Calcination: Heat the pre-oxidized fiber to 400 °C at a rate of 3 °C / min under an argon atmosphere of 200 ml / min, and then pass H 2 / N 2 After the temperature reached 700 °C, the mixed gas was turned off, and the temperature was continued to rise to 1600 °C with argon ...

Embodiment 2

[0033] 1. Preparation of spinning solution: Weigh 1 g of alkali lignin, 1 g of PAN, 0.4 g of nickel acetate, 0.1 g of boric acid and 17 ml of DMF, stir on a magnetic stirrer at 25 °C until completely dissolved to form a uniform spinning solution.

[0034] 2. Preparation of composite fibers by electrospinning: under the conditions of voltage 22 kv, receiving distance 15 cm, spinning solution flow rate 0.5 ml / h, and electrospinning temperature 45 ℃, alkali lignin / PAN composite micro-nano was obtained by electrospinning Fibers were dried in a vacuum oven at 70 °C for 8 h.

[0035] 3. Pre-oxidation: The dried alkali lignin / PAN composite micro-nanofibers were pre-oxidized in a muffle furnace at 280 °C for 1 h in an air atmosphere.

[0036] 4. Calcination: Heat the pre-oxidized fiber to 400 °C at a rate of 3 °C / min under an argon atmosphere of 200 ml / min, and then pass H 2 / N 2 After the temperature reached 700 °C, the mixed gas was turned off, and the temperature was raised to 1...

Embodiment 3

[0039] 1. Prepare spinning solution: weigh 1 g of LN, 1 g of polyvinylpyrrolidone (PVP), 0.4 g of nickel acetate, 0.1 g of boric acid and 17 ml of DMF, stir on a magnetic stirrer at 25 °C until completely dissolved A homogeneous spinning solution is formed.

[0040] 2. Preparation of composite fibers by electrospinning: Under the conditions of voltage 18 kv, receiving distance 15 cm, spinning solution flow rate 0.8 ml / h, and electrospinning temperature 45 °C, LN / PVP composite micro-nano fibers were obtained by electrospinning, and placed Dry in a vacuum oven at 70 °C for 8 h.

[0041] 3. Pre-oxidation: The dried LN / PVP composite micro-nanofibers were pre-oxidized at 280 °C for 1 h in an air atmosphere in a muffle furnace.

[0042] 4. Calcination: Heat the pre-oxidized fiber to 400 °C at a rate of 3 °C / min under an argon atmosphere of 200 ml / min, and then pass H 2 / N 2 After the temperature reached 700 °C, the mixed gas was turned off, and the temperature was raised to 1600 ...

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Abstract

The invention relates to a method for preparing a hydrogen storage material, and particularly relates to a method for preparing a lignin-based carbon fiber hydrogen storage material by electrostatic spinning. The method comprises the following steps: preparing a sodium lignin sulfonate/polyacrylonitrile/nickel acetate/boric acid spinning solution; preparing sodium lignin sulfonate/polyacrylonitrile composite micro-nano fiber through electrostatic spinning; drying in a vacuum drying oven and pre-oxidizing in an air atmosphere in a muffle furnace; and gradually heating and calcining in a condition of continuously introducing an inert gas into the tubular furnace to obtain sodium lignin sulfonate/polyacrylonitrile composite carbon fiber containing a Ni-B catalyst, wherein Ni-B realizes an effect of catalytic graphitization. The prepared sodium lignin sulfonate/polyacrylonitrile composite carbon fiber has relatively high graphitization degree, and the hydrogen absorption capacity under the conditions of 298K and 95bar reaches 0.92wt% within 60s.

Description

technical field [0001] The invention relates to a method for preparing a hydrogen storage material, and in particular provides a method for preparing a lignin-based carbon fiber hydrogen storage material by an electrospinning method. Background technique [0002] Hydrogen energy has the advantages of environmental friendliness, abundant reserves, and high combustion calorific value, and is known as the most potential green energy in the 21st century. However, the lack of a safe, economical and effective storage technology is the current problem that restricts the practicality and scale of hydrogen energy. Therefore, the development of hydrogen storage materials with excellent performance is the key to solving the problem of hydrogen energy storage. [0003] Carbon-based hydrogen storage materials have the advantages of light weight and low cost, and have gradually attracted attention in recent years. The microstructure of graphite carbon fiber is composed of many graphite s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/17D01F9/22D01D5/00
Inventor 钱庆荣许丽洪许兢陈庆华曾令兴黄宝铨
Owner QUANGANG PETROCHEM RES INST OF FUJIAN NORMAL UNIV
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