A kind of preparation method of carbon fiber precursor lignin/polylactic acid fiber

A polylactic acid fiber and lignin technology, which is applied in the chemical characteristics of fibers, conjugated synthetic polymer rayon, conjugated rayon, etc., can solve the problems of high production cost, environmental pollution, difficulty in solvent recovery, and the like, Achieve low production costs, broad market prospects, and solve the effect of continuous production

Active Publication Date: 2017-06-06
DONGHUA UNIV
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Problems solved by technology

Patent CN 103748271 A discloses a method for manufacturing lignin-containing precursor fibers and carbon fibers. Continuous precursor fibers are obtained by solution spinning lignin and high polymers in an appropriate solvent, but the method used is solution spinning , the production cost is high, the solvent recovery is difficult, and at the same time, it causes certain pollution to the environment

Method used

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  • A kind of preparation method of carbon fiber precursor lignin/polylactic acid fiber
  • A kind of preparation method of carbon fiber precursor lignin/polylactic acid fiber

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Slice lignin powder and polylactic acid (M w =1.77×10 5 , PDI=1.3) at 190° C. and 80° C. in a vacuum oven for intermittent heat treatment, and the heat treatment time was 0.5 h and 8 h, respectively. Fully mix 495g of heat-treated lignin powder and 5g of heat-treated polylactic acid slices, and obtain lignin / polylactic acid composite masterbatch through twin-screw granulation. °C and 225 °C. Put the dried composite masterbatch into a melt spinning machine for spinning to obtain lignin / polylactic acid composite fibers. The spinning temperature is 200-240°C, the speed of the metering pump is 20rpm, the specification is 1.8cc / r, and the spinneret The specification is 0.18mm×12f, the spinning speed is 100m / min, and the draft ratio is 1.1 times. The obtained lignin / polylactic acid composite fiber is pre-oxidized (the pre-oxidation temperature is 270°C, the heating rate is 0.1°C / min, and the pre-oxidation time is 10min) and carbonized (the carbonization temperature is 1000...

Embodiment 2

[0025] Slice lignin powder and polylactic acid (Mw=1.77×10 5 , PDI=1.3) at 200° C. and 90° C. in a vacuum oven for intermittent heat treatment, and the heat treatment time was 1 h and 6 h, respectively. Fully mix 475g of heat-treated lignin powder and 25g of heat-treated polylactic acid slices, and obtain lignin / polylactic acid composite masterbatch through twin-screw granulation. °C and 220 °C. Put the dried composite masterbatch into a melt spinning machine for spinning to obtain lignin / polylactic acid composite fibers. The spinning temperature is 200-240°C, the speed of the metering pump is 20rpm, the specification is 1.8cc / r, and the spinneret The specification is 0.18mm×12f, the spinning speed is 300m / min, and the draft ratio is 1.2 times. The obtained lignin / polylactic acid composite fiber is pre-oxidized (the pre-oxidation temperature is 280°C, the heating rate is 0.1°C / min, and the pre-oxidation time is 10min) and carbonized (the carbonization temperature is 1000°C, ...

Embodiment 3

[0027] Lignin powder and polylactic acid slices (Mw=1.77×105, PDI=1.3) were subjected to intermittent heat treatment in a vacuum oven at 210°C and 100°C for 2h and 10h, respectively. Fully mix 450g of heat-treated lignin powder and 50g of heat-treated polylactic acid slices, and obtain lignin / polylactic acid composite masterbatch through twin-screw granulation. °C and 215 °C. Put the dried composite masterbatch into a melt spinning machine for spinning to obtain lignin / polylactic acid composite fibers. The spinning temperature is 200-230°C, the speed of the metering pump is 30rpm, the specification is 1.8cc / r, and the spinneret The specification is 0.18mm×12f, the spinning speed is 500m / min, and the draft ratio is 1.3 times. The obtained lignin / polylactic acid composite fiber was preoxidized (the preoxidation temperature was 290°C, the heating rate was 0.2°C / min, and the preoxidation time was 10min) and carbonized (the carbonization temperature was 1000°C, and the heating rat...

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Abstract

The invention relates to a method for preparing a carbon fiber precursor lignin / polylactic acid fiber. The method comprises the following steps: carrying out intermittent heat treatment on purified lignin powder and polylactic acid slices in a vacuum drying oven; mixing the lignin powder subjected to heat treatment with the polylactic acid slices; pelleting at 160-250 DEG C through double screw rods to obtain lignin / polylactic acid composite master batches; and spinning the dried lignin / polylactic acid composite master batches at 190-250 DEG C through a melt-spinning machine, so as to obtain the carbon fiber precursor lignin / polylactic acid fiber. The carbon fiber precursor lignin / polylactic acid fiber provided by the invention has the advantages of renewable raw materials, excellent fiber quality, small diameter of obtained fiber, high strength and low cost; continuous production can be carried out; the carbon fiber precursor lignin / polylactic acid fiber is expected to be applied to the fields such as automobiles, high-speed rails, buildings and sports goods as a reinforcing material after being carbonized; and the market prospect is wide.

Description

technical field [0001] The invention belongs to the field of preparation of carbon fiber precursors, in particular to a preparation method of carbon fiber precursor lignin / polylactic acid fibers. Background technique [0002] Carbon fiber is widely used in high-end fields such as aerospace and national defense construction due to its excellent mechanical properties and service performance, but it is rarely involved in a large number of civilian fields. The main reason is that the cost of producing carbon fiber is relatively high. Developing low-cost carbon fiber and expanding its application in the civil market has become the future development direction. As a by-product of papermaking black liquor, lignin has become an ideal material for the preparation of low-cost carbon fibers due to its wide source of raw materials, renewable resources, low price, and rich benzene ring structure. Patent CN 103140539 A discloses thermoplastic lignin for the production of carbon fibers, b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F8/14D01F8/18D01F9/26D01F9/17
Inventor 朱美芳王世超左伟伟李妍李健相恒学周哲
Owner DONGHUA UNIV
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