PREPARATION OF ISOTROPIC PRECURSORS FROM

ZERO QI TSL PITCH

Shubhashis Adak
Experimental Method of Precursor Preparation

Objective: Preparation of isotropic precursor from zero QI TSL pitch for carbon fiber preparation.

Materials used: Zero QI Coal tar pitch (TSL, holding time: 1 h at 350 OC), Perchloric acid (60%)

Schematic of Experimental Procedure

Heat
Reacted at Washed Treatment
CTP 100-150 oC with water in Tube
Feedstock for Precursor
for 30 mins Reaction and dried Furnace
Heat for melt
Mixture Treatment spinning
HClO4

Perchloric Heat Treatment Condition

Experimental Conditions: Acid
Temperature Heating Rate Soaking Time N2 /Air Flow
Concentration
(oC) (oC/min) (h) Rate
(w/w)%
(Litre/min)

1 290-340 3 1-2 3/1

Nomenclature: Coal tar pitch (CTP)…..Perchloric acid (A)----Heat treatment temperature…..Soaking time
Optical Texture of Raw Pitch

(1) TSL PITCH (2) TSL PITCH

(5) NMP Distilled TSK Pitch

(3) ZERO QI TSL PITCH (4) ) ZERO QI TSL PITCH

Optical Texture of Perchloric acid treated Pitch

Sample ID Softening Point

(oC)
CTP 82.0

CTP-A 1O3.7

(1) CTP (2) CTP

(3) CTP-A (4) CTP-A

 Optical Texture of Perchloric acid and Heat treated Pitch

Sl No. Sample ID S.P (oC)

1 CTP-A-290-1 173.4
2 CTP-A-300-1 175.2

3 CTP-A-300-2 179.8

4 CTP-A-310-1 199.2
5 CTP-A-320-1 203.9
TI= 60.73% (1) CTP-A-300-2 (2) CTP-A-300-2
NMPI=2.92%

6 CTP-A-330-1 206.2
7 CTP-A-340-2 243.9
8 CTP-320-1 152.7
9 CTP-320-1(Air) 197.3
10 CTP-A-320- 208.5
1(Air) (3) CTP-A-310-1 (4) CTP-A-320-1
Conclusions

Isotropic precursors having suitable softening point and insoluble content

favourable for melt spinning have been produced by perchloric acid treatment
and simultaneous heat treatment.