JPH0440450B2 - - Google Patents
Info
- Publication number
- JPH0440450B2 JPH0440450B2 JP62243292A JP24329287A JPH0440450B2 JP H0440450 B2 JPH0440450 B2 JP H0440450B2 JP 62243292 A JP62243292 A JP 62243292A JP 24329287 A JP24329287 A JP 24329287A JP H0440450 B2 JPH0440450 B2 JP H0440450B2
- Authority
- JP
- Japan
- Prior art keywords
- carbon
- laser
- reaction
- gas
- compounds
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 47
- 239000004917 carbon fiber Substances 0.000 claims description 47
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 32
- 239000003054 catalyst Substances 0.000 claims description 22
- 150000001722 carbon compounds Chemical class 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 21
- 239000002994 raw material Substances 0.000 claims description 20
- 238000004519 manufacturing process Methods 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 14
- -1 ethylene, ethylene Chemical group 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 239000000835 fiber Substances 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 238000000151 deposition Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 description 62
- 239000007789 gas Substances 0.000 description 29
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 25
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 23
- 239000005977 Ethylene Substances 0.000 description 23
- 238000010521 absorption reaction Methods 0.000 description 13
- 239000012159 carrier gas Substances 0.000 description 13
- 150000001875 compounds Chemical class 0.000 description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 229910052742 iron Inorganic materials 0.000 description 8
- 150000003623 transition metal compounds Chemical class 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 239000010419 fine particle Substances 0.000 description 6
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 239000011593 sulfur Substances 0.000 description 5
- 229910052717 sulfur Inorganic materials 0.000 description 5
- 150000002484 inorganic compounds Chemical class 0.000 description 4
- 229910010272 inorganic material Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 150000002894 organic compounds Chemical class 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 229910017052 cobalt Inorganic materials 0.000 description 3
- 239000010941 cobalt Substances 0.000 description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 3
- 238000007380 fibre production Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 229910052763 palladium Inorganic materials 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical group [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- 150000003624 transition metals Chemical class 0.000 description 3
- FCEHBMOGCRZNNI-UHFFFAOYSA-N 1-benzothiophene Chemical compound C1=CC=C2SC=CC2=C1 FCEHBMOGCRZNNI-UHFFFAOYSA-N 0.000 description 2
- YBYIRNPNPLQARY-UHFFFAOYSA-N 1H-indene Chemical compound C1=CC=C2CC=CC2=C1 YBYIRNPNPLQARY-UHFFFAOYSA-N 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 2
- JDMMZVAKMAONFU-UHFFFAOYSA-N 2-trimethylsilylacetic acid Chemical compound C[Si](C)(C)CC(O)=O JDMMZVAKMAONFU-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 description 2
- 150000007824 aliphatic compounds Chemical class 0.000 description 2
- LPIQUOYDBNQMRZ-UHFFFAOYSA-N cyclopentene Chemical compound C1CC=CC1 LPIQUOYDBNQMRZ-UHFFFAOYSA-N 0.000 description 2
- 230000020169 heat generation Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 150000001283 organosilanols Chemical class 0.000 description 2
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 238000013341 scale-up Methods 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- RMVRSNDYEFQCLF-UHFFFAOYSA-N thiophenol Chemical compound SC1=CC=CC=C1 RMVRSNDYEFQCLF-UHFFFAOYSA-N 0.000 description 2
- 239000011882 ultra-fine particle Substances 0.000 description 2
- 238000001947 vapour-phase growth Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- MHBOFSJQAKACCM-UHFFFAOYSA-N 1,1,2,2,3,3,4,4-octakis-phenyltetrasiletane Chemical compound C1=CC=CC=C1[Si]1(C=2C=CC=CC=2)[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)[Si]1(C=1C=CC=CC=1)C1=CC=CC=C1 MHBOFSJQAKACCM-UHFFFAOYSA-N 0.000 description 1
- DNVUQRLSJFZVBN-UHFFFAOYSA-N 1-phenyl-1,3,5,2,4,6-triazatrisilinane Chemical compound N1[SiH2]N[SiH2]N([SiH2]1)c1ccccc1 DNVUQRLSJFZVBN-UHFFFAOYSA-N 0.000 description 1
- HRQDDZWMEGEOOO-UHFFFAOYSA-N 2-trimethylsilylpropanoic acid Chemical compound OC(=O)C(C)[Si](C)(C)C HRQDDZWMEGEOOO-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- LVZWSLJZHVFIQJ-UHFFFAOYSA-N Cyclopropane Chemical compound C1CC1 LVZWSLJZHVFIQJ-UHFFFAOYSA-N 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 241000779819 Syncarpia glomulifera Species 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- RQVFGTYFBUVGOP-UHFFFAOYSA-N [acetyloxy(dimethyl)silyl] acetate Chemical compound CC(=O)O[Si](C)(C)OC(C)=O RQVFGTYFBUVGOP-UHFFFAOYSA-N 0.000 description 1
- APDDLLVYBXGBRF-UHFFFAOYSA-N [diethyl-(triethylsilylamino)silyl]ethane Chemical compound CC[Si](CC)(CC)N[Si](CC)(CC)CC APDDLLVYBXGBRF-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 125000002947 alkylene group Chemical group 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 125000006267 biphenyl group Chemical group 0.000 description 1
- RLECCBFNWDXKPK-UHFFFAOYSA-N bis(trimethylsilyl)sulfide Chemical compound C[Si](C)(C)S[Si](C)(C)C RLECCBFNWDXKPK-UHFFFAOYSA-N 0.000 description 1
- 229960000411 camphor oil Drugs 0.000 description 1
- 239000010624 camphor oil Substances 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000002134 carbon nanofiber Substances 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- RLTCOMJEWHDYIO-UHFFFAOYSA-N chloro-difluoro-methylsilane Chemical compound C[Si](F)(F)Cl RLTCOMJEWHDYIO-UHFFFAOYSA-N 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 125000000753 cycloalkyl group Chemical group 0.000 description 1
- 239000010727 cylinder oil Substances 0.000 description 1
- XYWDPYKBIRQXQS-UHFFFAOYSA-N di-isopropyl sulphide Natural products CC(C)SC(C)C XYWDPYKBIRQXQS-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- DAKRXZUXJUPCOF-UHFFFAOYSA-N diethyl(dihydroxy)silane Chemical compound CC[Si](O)(O)CC DAKRXZUXJUPCOF-UHFFFAOYSA-N 0.000 description 1
- TTZNCSDPSRUFNZ-UHFFFAOYSA-N diisocyanato(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](N=C=O)(N=C=O)C1=CC=CC=C1 TTZNCSDPSRUFNZ-UHFFFAOYSA-N 0.000 description 1
- UBHZUDXTHNMNLD-UHFFFAOYSA-N dimethylsilane Chemical compound C[SiH2]C UBHZUDXTHNMNLD-UHFFFAOYSA-N 0.000 description 1
- LTYMSROWYAPPGB-UHFFFAOYSA-N diphenyl sulfide Chemical compound C=1C=CC=CC=1SC1=CC=CC=C1 LTYMSROWYAPPGB-UHFFFAOYSA-N 0.000 description 1
- 238000005367 electrostatic precipitation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003623 enhancer Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 125000005677 ethinylene group Chemical group [*:2]C#C[*:1] 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 239000003502 gasoline Substances 0.000 description 1
- 239000012208 gear oil Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 150000002391 heterocyclic compounds Chemical class 0.000 description 1
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical class II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 150000002540 isothiocyanates Chemical class 0.000 description 1
- XLTUPERVRFLGLJ-UHFFFAOYSA-N isothiocyanato(trimethyl)silane Chemical compound C[Si](C)(C)N=C=S XLTUPERVRFLGLJ-UHFFFAOYSA-N 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- POPACFLNWGUDSR-UHFFFAOYSA-N methoxy(trimethyl)silane Chemical compound CO[Si](C)(C)C POPACFLNWGUDSR-UHFFFAOYSA-N 0.000 description 1
- GIGVICQLYWGMGW-UHFFFAOYSA-N methyl(triphenyl)silane Chemical compound C=1C=CC=CC=1[Si](C=1C=CC=CC=1)(C)C1=CC=CC=C1 GIGVICQLYWGMGW-UHFFFAOYSA-N 0.000 description 1
- WXEHBUMAEPOYKP-UHFFFAOYSA-N methylsulfanylethane Chemical compound CCSC WXEHBUMAEPOYKP-UHFFFAOYSA-N 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 150000001282 organosilanes Chemical class 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 125000005375 organosiloxane group Chemical group 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000010665 pine oil Substances 0.000 description 1
- 239000001739 pinus spp. Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 150000003431 steroids Chemical group 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- UVVUGWBBCDFNSD-UHFFFAOYSA-N tetraisocyanatosilane Chemical class O=C=N[Si](N=C=O)(N=C=O)N=C=O UVVUGWBBCDFNSD-UHFFFAOYSA-N 0.000 description 1
- CZDYPVPMEAXLPK-UHFFFAOYSA-N tetramethylsilane Chemical compound C[Si](C)(C)C CZDYPVPMEAXLPK-UHFFFAOYSA-N 0.000 description 1
- JTNXQVCPQMQLHK-UHFFFAOYSA-N thioacetone Chemical compound CC(C)=S JTNXQVCPQMQLHK-UHFFFAOYSA-N 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- XEJUFRSVJVTIFW-UHFFFAOYSA-N triethyl(triethylsilyl)silane Chemical compound CC[Si](CC)(CC)[Si](CC)(CC)CC XEJUFRSVJVTIFW-UHFFFAOYSA-N 0.000 description 1
- MKMPBMJIGMMCPB-UHFFFAOYSA-N triethylsilylformonitrile Chemical compound CC[Si](CC)(CC)C#N MKMPBMJIGMMCPB-UHFFFAOYSA-N 0.000 description 1
- OJAJJFGMKAZGRZ-UHFFFAOYSA-N trimethyl(phenoxy)silane Chemical compound C[Si](C)(C)OC1=CC=CC=C1 OJAJJFGMKAZGRZ-UHFFFAOYSA-N 0.000 description 1
- ZMHATUZXFSOVSC-UHFFFAOYSA-N triphenyl(triphenylsilyl)silane Chemical compound C1=CC=CC=C1[Si]([Si](C=1C=CC=CC=1)(C=1C=CC=CC=1)C=1C=CC=CC=1)(C=1C=CC=CC=1)C1=CC=CC=C1 ZMHATUZXFSOVSC-UHFFFAOYSA-N 0.000 description 1
- AKQNYQDSIDKVJZ-UHFFFAOYSA-N triphenylsilane Chemical compound C1=CC=CC=C1[SiH](C=1C=CC=CC=1)C1=CC=CC=C1 AKQNYQDSIDKVJZ-UHFFFAOYSA-N 0.000 description 1
- NLSXASIDNWDYMI-UHFFFAOYSA-N triphenylsilanol Chemical compound C=1C=CC=CC=1[Si](C=1C=CC=CC=1)(O)C1=CC=CC=C1 NLSXASIDNWDYMI-UHFFFAOYSA-N 0.000 description 1
- KHQZLUVCZCAMFU-UHFFFAOYSA-N tripropyl(tripropylsilyloxy)silane Chemical compound CCC[Si](CCC)(CCC)O[Si](CCC)(CCC)CCC KHQZLUVCZCAMFU-UHFFFAOYSA-N 0.000 description 1
- FNRQRIRGNYNSHU-UHFFFAOYSA-N tripropylsilyl acetate Chemical compound CCC[Si](CCC)(CCC)OC(C)=O FNRQRIRGNYNSHU-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229940036248 turpentine Drugs 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/127—Carbon filaments; Apparatus specially adapted for the manufacture thereof by thermal decomposition of hydrocarbon gases or vapours or other carbon-containing compounds in the form of gas or vapour, e.g. carbon monoxide, alcohols
- D01F9/1271—Alkanes or cycloalkanes
- D01F9/1272—Methane
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/127—Carbon filaments; Apparatus specially adapted for the manufacture thereof by thermal decomposition of hydrocarbon gases or vapours or other carbon-containing compounds in the form of gas or vapour, e.g. carbon monoxide, alcohols
- D01F9/1273—Alkenes, alkynes
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/127—Carbon filaments; Apparatus specially adapted for the manufacture thereof by thermal decomposition of hydrocarbon gases or vapours or other carbon-containing compounds in the form of gas or vapour, e.g. carbon monoxide, alcohols
- D01F9/133—Apparatus therefor
Description
［産業上の利用分野］
本発明は炭素繊維の製造方法に係り、特にレー
ザビームを利用して気相成長法により炭素繊維を
高収率で製造する方法に関する。
［従来の技術］
炭素繊維は、従来らかPAN系、ピツチ系のも
のが商業生産されている。しかし、PAN系は高
価であり、ピツチ系はプロセスが複雑で品質の制
御がむずかしいなどの致命的な欠点がある。
一方、近年気相成長法が提案されている。従
来、気相成長炭素繊維は、電気炉内にアルミナな
どの磁器、黒鉛などの基板を置き、これに炭素成
長核、鉄、ニツケルなどの超微粒子触媒を形成せ
しめ、この上にベンゼンなどの炭化水素のガスと
水素キヤリヤガスの混合ガスを導入し、950〜
1300℃の温度下に炭化水素を分解せしめることに
より、基板上に炭素繊維を成長させる方法が知ら
れている。
しかし、このような方法では、基板表面の微
妙な温度ムラや、周囲の繊維の密生度によつて長
さの不均一が起り易いこと、また炭素の供給源
としてのガスが反応によつて消費されることによ
り反応管の入口に近い所と出口に近い所で繊維径
が相当異なること、基板表面でのみ生成が行な
われるため、反応管の中心部分は反応に関与せず
収率が悪いこと、超微粒子の基板への分散、還
元、成長次いで繊維の取出しという独立に実施を
必要とするプロセスがあるため、連続製造が不可
能であり、従つて生産性が悪いなどの問題点を有
する。
そこで、炭素化合物のガスと無機もしくは有機
遷移金属化合物のガスとキヤリヤガスとの混合ガ
スを高温反応させる炭素繊維の製造方法が提案さ
れた（特開昭60−54998，60−224816など）。
［発明が解決しようとする問題点］
しかしながら、特開昭60−54998，60−224816
などの方法では、反応容器も加熱されるところか
ら、器壁に副生物が付着し、収率が低下したり、
連続運転が困難である等の問題が生じていた。ま
た、スケールアツプも容易ではなく、大量生産に
不向きである、あるいは加熱に電気炉を使用して
おり、エネルギーコストが高い等の問題があつ
た。
［問題点を解決するための手段］
本発明は上記の問題を解決し、低コストで効率
的に炭素繊維を製造する方法を提供するものであ
る。
本発明の炭素繊維の製造方法は、レーザ照射下
において、原料の炭素化合物のガスと、浮遊状態
にある接触粒子とを接触させて炭素を繊維状に析
出させる方法であつて、レーザとしてCO2レーザ
を用いると共に、原料として、エチレン以外の炭
素化合物に対して、エチレンを10〜50体積％含む
混合原料を用いることを特徴とする。
即ち、本発明者らは、従来の問題点を解決する
べく鋭意検討を重ねた結果、
レーザ照射下において、炭素化合物のガスと、
浮遊状態にある触媒粒子とを接触させて炭素を繊
維状に析出させることを特徴とする炭素繊維の製
造方法、
及び、この方法の実施に好適な装置として、
内部を反応ゾーンとする反応容器と、
該反応ゾーンへ向けてレーザビームを照射する
レーザ装置と、
該反応ゾーンを挟んで反応容器の一方の側に連
設されたキヤリアガスの導入手段、炭素化合物ガ
スの導入手段及び触媒粒子又は触媒原料ガスの導
入手段と、
該反応ゾーンを挟んで反応容器の他方の側に連
設された炭素繊維の捕集手段と、を備えたことを
特徴とする炭素繊維の製造装置、
を開発し、本出願人より先に特許出願した（特願
昭61−234896号。以下「先願」という。）
本発明者らは、上記先願の方法において、エネ
ルギー効率をより向上させるべく更に研究を重ね
た結果、レーザとしてCO2レーザを用い、また原
料の炭素化合物としてエチレンを含むものを用い
ることにより、著しく優れた効果が得られること
を見出し、本発明を完成させた。
以下、本発明についてさらに詳細に説明する。
本発明における炭素化合物原料は、エチレン以
外のガス化可能な炭素化合物全般とエチレンとの
混合原料である。エチレン以外の炭素化合物（以
下、単に「炭素化合物」ということがある。）と
しては、CCl4，CHCl3，CH2Cl2，CH3Cl，CO，
CS2等の無機化合物と有機化合物全般が挙げられ
る。これらのうち、特に有用性の高い化合物は、
脂肪族炭化水素、芳香族炭化水素である。また、
これらの他、窒素、酸素、硫黄、弗素、沃素、
燐、砒素等の元素を含んだ誘導体も使用可能であ
る。具体的な個々の化合物の例の一部を挙げる
と、メタン（天然ガスでも良い。）、エタン等のア
ルカン化合物、ブタジエン等のエチレンを除くア
ルケン化合物、アセチレン等のアルキレン化合
物、ベンゼン、トルエン、スチレン等のアリール
炭化水素化合物、インデン、ナフタリン、フエナ
ントレン等の縮合環を有する芳香族炭化水素、シ
クロプロパン、シクロヘキサン等のシクロパラフ
イン化合物、シクロペンテン、シクロヘキサン等
のシクロオレフイン化合物、ステロイド等の縮合
環を有する脂環式炭化水素化合物、メチルチオー
ル、メチルエチルスルフイド、ジメチルチオケト
ン等の含硫黄脂肪族化合物、フエニルチオール、
ジフエニルスルフイド等の含硫黄芳香族化合物、
ベンゾチオフエン、チオフエン等の含硫黄複素環
式化合物、また単体ではないガソリン等の消防法
危険物第四類、第一石油類、ケロシン、テレピン
油、樟脳油、松根油等の第二石油類、重油等の第
三石油類、ギヤー油、シリンダ油等の第四石油類
も有効に使用できる。また、これら混合物も使用
できることは言うに及ばない。
このようなエチレン以外の炭素化合物とエチレ
ンとの混合割合は、エチレン以外の炭素化合物に
対するエチレンの体積比で10〜50％とする。この
エチレンの割合が10％未満では、エチレン使用に
よる十分なエネルギー効率改善効果が得られず、
50％を超えるとエネルギーが過剰となり、反応域
の温度が高くなりすぎるなど、反応条件が悪くな
り、収率の向上が望めなくなる。
本発明において、触媒としては、無機遷移金属
化合物、Siの無機化合物、有機遷移金属化合物、
Siの有機化合物などが挙げられる。この無機遷移
金属化合物とは、単独で気化が可能な遷移金属の
無機化合物又は水もしくは少なくとも一種以上の
水もしくは有機溶媒（この有機溶媒としては炭素
原料化合物を用いても良い。）に可溶なもしくは
微粒子として懸濁可能な遷移金属の無機化合物が
対象となる。遷移金属としては、鉄、ニツケル、
コバルト、モリブデン、バナジアム、パラジウム
等が好ましく、特に鉄が好ましい。即ち、本発明
で用いるCO2レーザは、特に鉄触媒を振動励起す
る作用に優れ、触媒の高活性化が図れるのであ
る。前者の単独で気化が可能な無機遷移金属化合
物としては、Fe（NO）4，FeCl3，Fe（NO）3Cl，
Fe（NO）2，Fe（NO）2Ｉ，FeF3等が挙げられる。
また後者としては、前者として挙げた化合物の他
に、Fe（NO3）2，FeBr3，Fe（HCOO）3，C27H42
FeN9O12，Fe（SO4）3，Fe（SCN）3，Fe（NO）3
NH3，Co（NO）2Cl，Ni（NO）Cl，Pd（NO）2Cl2，
NiCl2等が代表として挙げられる。
本発明における有機遷移金属化合物とは、アル
キル基と金属が結合したアルキル金属、アリル基
と金属が結合したアリル錯体、炭素間２重結合や
３重結合と金属とが結合したπ−コンプレツクス
とキレート型化合物等に代表される有機遷移金属
化合物である。また、ここで遷移金属としては、
スカンジウム、チタン、パナジウム、クロム、マ
ンガン、鉄、コバルト、ニツケル、イツトリウ
ム、ジルコニウム、ニオブ、モリブデン、ルテニ
ウム、ロジウム、パラジウム、タンタル、タング
ステン、レニウム、イリジウム、白金を指すもの
であるが、これらの内、特に周期律表族に属す
るもの、その内で特に鉄、ニツケル、コバルトが
好適であつて、前述の理由から鉄が最も好適であ
る。
また、含硫黄炭素化合物または無機硫黄化合物
の存在下では、シリコンの無機化合物も用いるこ
とができる。例えば、上記の無機金属化合物にお
いて金属をSiに置換したものや炭化珪素を用い得
る。さらに、各種の有機珪素化合物をも用い得
る。
有機珪素化合物としては、珪素−炭素結合をも
つ有機化合物の他にシラン、ハロゲンシランを便
宜上含むものとする。炭素−珪素結合を持つ有機
化合物としては、テトラメチルシラン、メチルト
リフエニルシラン等のオリガノシラン、クロルジ
フルオルメチルシラン、プロムトリプロピルシラ
ン等のオルガノハロゲンシラン；メトキシトリメ
チルシラン、トリメチルフエノキシシラン等のオ
ルガノアルコキシシラン；ジアセトキシジメチル
シラン、アセトキシトリプロピルシラン等のオル
ガノアセトキシシラン；ヘキサエチルジシラン、
ヘキサフエニルジシラン、オクタフエニルシクロ
テトラシラン等のオルガノポリシラン；ジメチル
シラン、トリフエニルシラン等のオルガノヒドロ
ゲノシラン；（SiH2）oで表示されるシクロシラ
ン；トリフエニルシラザン、ヘキサエチルジシラ
ザン、ヘキサフエニルシクロトリシラザン等のオ
ルガノシラザン、（SiH2HN）oで表示されるシク
ロシラザンジエチルシランジオール、トリフエニ
ルシラノール等のオルガノシラノール；トリメチ
ルシリル酢酸、トリメチルシリルピロピオン酸等
のオルガノシラノール；トリメチルシリル酢酸、
トリメチルシリルプロピオン酸、ジフエニルシリ
コンジイソチオシアナート等のオルガノシランカ
ルボン酸；トリメチルシリコンイソシアナート、
ジフエニルシリコンジイソシアナート等のシリコ
ンイソシアナート；トリメチルシリコンイソチオ
シアナート等のオルガノシリコンイソチオシアナ
ート；シアン化トリエチルシリル等のオルガノシ
リコンエステル；ヘキサメチルジシルチアン、テ
リラメチルシクロジシルチアン等のシルチアン；
（SiH2Ｓ）oで表示されるシクロシルチアン；ヘキ
サメチルジシルメチレン、オクタメチルトリシル
メチレン等のオルガノシルメチレン；ヘキサメチ
ルジシロキサン、ヘキサプロピルジシロキサン等
のオルガノシロキサン等が挙げられるが、その他
の炭素−珪素結合を含む化合物であつてもよい。
また、これらの混合物の使用も可能である。
なお、本発明では、予め微粒子として生成され
た触媒粒子（例えば乾燥した微粉末）を反応容器
内に導入するようにしても良い。
本発明におけるキヤリアガスとは、直接反応に
関与しないガス全般を対象としている。例示すれ
ば、H2ガス、N2ガス、NH3ガス、Arガス、He
ガス、Krガス、又はこれらの混合ガスを主体と
するガスである。このうち、H2ガスが通常の場
合用いられる。
また、キヤリアガスなど、容器内に導入される
ガスにレーザの吸収効果を高めるための成分を添
加しても良い。この場合、添加成分は使用するレ
ーザの波長により適宜選択され、本発明で用いる
CO2レーザに対してはNH3やC2H4をレーザ吸収
効果向上剤として添加することができる。
以下本発明について図面に示す好適な態様を参
照しながら詳細に説明する。
第１図は本発明を実施するに好適な装置の一例
を示す概略的な断面図である。符号１０は反応容
器（本例では反応管）であり、その一端側にCO2
レーザビームを照射するためのCO2レーザ発振器
１２が設置され、他端側にはレーザ吸収板１４が
設置されている。また、前記一端側には、触媒粒
子となる物質を含む化合物の供給用配管１６と、
キヤリアガスの供給用配管１８と、エチレンと炭
素化合物との混合原料のガスを供給するための配
管２０とが接続され、これら配管１６，１８，２
０の途中にそれぞれ流量制御装置１６ａ，１８
ａ，２０ａが設けられている。
また、反応管１０の他端側には炭素繊維捕集器
２２が接続され、この炭素繊維捕集器２２には排
ガスの抜出管２４が接続されている。
上記の如く構成された炭素繊維製造装置におい
て、反応容器内に導入された触媒粒子となる物質
を含む化合物は、CO2レーザビームによつて励起
されて分解し、遷移元素又はSiCなどの触媒粒子
（通常の粒径は0.1〜10μｍ程度である）が生成す
る。更に、CO2レーザビームによつて励起、分解
された原料の炭素化合物がこの微粒子上に析出
し、炭素繊維が成長する。この際、原料中に存在
するエチレンがCO2レーザビームの光子エネルギ
ー吸収により励起発熱し、反応帯域の温度を約
1000℃程度に上昇させ、炭素繊維生成条件が達成
される。
本発明において、微粒子が生成し、これを成長
点として炭素繊維が生成する反応容器の器壁の温
度は、従来の外熱式の電気炉を用いた反応容器の
それよりも相当に低く、器壁に副生物を付着する
ことはない。従つて、本発明では、反応容器の材
質を高価な高耐食性あるいは高耐熱性のものに限
定する必要はない。また、レーザビームを採用し
ているので、一般の外熱式の電気炉よりもエネル
ギー消費が少なく、エネルギーコストが低廉であ
る。ただし、本発明では必要に応じ外熱式の電気
炉等の外部加熱手段を、反応容器を取り巻くよう
に設け、反応ゾーンの器壁を加熱してもよい。こ
の場合、器壁への生成物の付着を防止するため
に、器壁温度が600℃未満とりわけ550℃以下とな
るように外部加熱するのが好適である。
本発明において、触媒粒子の大きさ或いは炭素
繊維の直径及び長さ等は、原料ガスの分圧、滞留
時間、レーザ強度等を制御することによつて調節
が可能である。
反応容器内における反応の順序は、上述の如く
触媒微粒子の生成、炭素繊維の成長となるのであ
るが、反応容器内を特に微粒子生成ゾーンと炭素
繊維成長ゾーンとにあえて分割する必要はない。
ただし、必要により上記の如く適当な外部加熱手
段を併設すること等により、炭素繊維成長ゾーン
を形成するようにしてもよい。
反応容器内において生成した炭素繊維は、キヤ
リアガスと共に炭素繊維捕集器２２内に導入され
る。この捕集方法は従来から知られている重力沈
降法、電気集塵法等の各種方法を採用することが
できる。なお、炭素繊維捕集器２２は、生成した
炭素繊維を冷却する役割をも果たす。
本発明によれば、通常長さ10μｍ〜500mm程度
であり、直径が0.1〜300μｍ程度の炭素繊維を容
易に製造することができる。
炭素繊維捕集器２２から抜き出されたキヤリア
ガスは、そのまま排気処理手段に導入して放出し
てもよいのであるが、精製後再循環させて用いる
ようにしてもよい。
上記の装置では、反応管１０の端部にレーザ吸
収板（例えば水冷銅板）１４を設置しているが、
光路長が短い場合などでは反射板を置いてレーザ
ビームの光路長を長くするように構成してもよ
い。
第２図は本発明の実施に好適な炭素繊維製造装
置の他の例の構成を示す概略的な断面図である。
符号３０は反応容器であり、本例では反応管３
２，３４，３６，３８を四角形の枠状に接続して
組み立ててある。そして、この四角形の隅角部に
はそれぞれプリズム３９を設けると共に、反応管
３２と３８との隅角部にはCO2レーザ発振器１２
を設置してある。また、この反応管３２と３８の
接続部にはZoSeなどCO2レーザビームのみを透過
させる窓板が設けられており、反応管３２と３８
とを遮断している。同様の窓板４２は反応管３４
と３６との接続部にも配置されている。
反応管３２と３６の一端側には、それぞれ触媒
粒子となる物質を含む化合物の供給用配管１６，
キヤリヤガスの供給用配管１８、エチレンと炭素
化合物との混合原料の供給用配管２０がそれぞれ
接続されており、これら配管の途中には流量制御
装置１６ａ，１８ａ，２０ａが設けられている。
また、反応管３４の反応管３６側の端部及び反
応管３８の反応管３２側の端部にはそれぞれ炭素
繊維捕集器２２ａ，ｂが接続され、該捕集器２２
ａ，ｂには排ガス抜出口２４が接続されている。
このように構成された第２図の装置において、
配管１６，１８及び２０から導入されたガスが反
応管３２，３４内で反応し炭素繊維を生成させ、
この炭素繊維は捕集器２２ａにて捕集される。ま
た、反応管３６，３８内にて生じた炭素繊維は、
同様に捕集器２２ｂで捕集される。この第２図の
装置では、CO2レーザビームの光路長が大きく、
効率よく炭素繊維を製造できる。なお、上記実施
例では四角形状に反応管を接続して反応容器を構
成しているが、これは五角形、六角形など他の形
状としてもよい。また、つづら折状に往復させる
接続方式や、反応管を並列的に配置したマルチ式
の接続方式など各種の接続方式を採用してもよ
い。
第３図は本発明の実施に好適な炭素繊維製造装
置の異なる構成例を示す斜視図である。この装置
では２枚の平板４０，４２と、レーザ反射板４
４，４６及びレーザ吸収板４８で反応容器５０を
構成してある。この反応容器５０においては、ガ
ス導入側５０ａから、エチレンと炭素化合物の混
合ガス、キヤリアガス及び触媒粒子となる物質を
含む化合物のガスが導入され、CO2レーザ発振器
１２がレーザ反射板４４に向けてレーザを照射し
ている。このCO2レーザは、反射板４４と４６と
の間で複数回反射され、やがてレーザ吸収板４８
で吸収されるが、この途中において上記のガスを
励起させ、炭素繊維を生成させる。生成した炭素
繊維は、キヤリアガス及び残余の原料ガス等と共
に反応容器５０の出口側５０ｂから排出され、炭
素繊維は適宜の捕集手段にて捕集される。
なお、CO2レーザ発振器１２は反応容器５０の
長手方向に首を振るように運動させてもよい。こ
のようにすれば反応容器５０内をくまなくCO2レ
ーザビームにて照射することができ、炭素繊維生
成反応が一層促進されている。
また、CO2レーザ発振器１２を首振り運動させ
る代りに、CO2レーザ発振器１２としてレーザビ
ームを拡散方向に照射するものを用いてもよい。
この場合には反応容器５０内のレーザ吸収板設置
部以外を全て鏡面としレーザビームを反射させる
必要がある。また、レーザ反射板４４として曲面
鏡を採用することにより、該レーザ反射板４４に
向けてレーザ光束を放射させるようにしてもよ
い。この場合でも、レーザ吸収板以外の部分の反
応容器内面を鏡面とする必要がある。
［作用］
CO2レーザは、鉄触媒等の触媒を効率的に振動
励起させ、高活性を発現させる作用が特に優れ
る。
一方、エチレンはCO2レーザの約10.6μｍの波
長域に吸収帯を持つため、原料中に特定割合のエ
チレンを混合させることにより、エチレンの光子
エネルギー吸収により発熱が起こり、反応域の温
度を容易に約1000℃の炭素繊維生成温度条件とす
ることが可能である。
このため、本発明の方法によれば、エネルギー
効率の向上が図れ、加熱温度の低温化、収率の向
上が達成される。
［実施例］
以下、好適な製造実施例について説明する。
実施例 １
第１図に示す装置において、下記の条件にて炭
素繊維の製造を行なつた。
レーザ：CO2レーザ（10.591μｍ）
混合原料：
メタン：チエレン＝100：30（体積比）
触媒粒子となる物質を含む化合物：
FeCl3水溶液
キヤリアーガス：H2
圧 力：常圧
滞留時間：１分
原料濃度：H2に対して5vol％
反応器：20mmID×450mmＬ
（石英製）
結果を第１表に示す。
実施例２〜４，比較例１〜３
混合原料のメタンとエチレンの体積比を第１表
に示す値としたこと以外は、実施例１と同様にし
て炭素繊維の製造を行なつた。
結果を第１表に示す。
第１表より明らかなように、本発明の方法によ
れば、高収率で炭素繊維を製造することができ
る。
なお、上記実施例１〜４において、いずれも器
壁への付着物は認められなかつた。
[Industrial Application Field] The present invention relates to a method for producing carbon fibers, and particularly to a method for producing carbon fibers at high yield by vapor phase growth using a laser beam. [Prior Art] Conventionally, PAN-based and Pitch-based carbon fibers have been commercially produced. However, PAN-based products are expensive, and pitch-based products have fatal drawbacks such as complicated processes and difficult quality control. On the other hand, a vapor phase growth method has been proposed in recent years. Conventionally, vapor-grown carbon fibers are produced by placing a substrate made of porcelain such as alumina or graphite in an electric furnace, forming carbon growth nuclei, ultrafine particle catalysts such as iron, and nickel on this, and then forming carbonization particles such as benzene on this. Introducing a mixed gas of hydrogen gas and hydrogen carrier gas, 950 ~
A method is known in which carbon fibers are grown on a substrate by decomposing hydrocarbons at a temperature of 1300°C. However, with this method, the length tends to be non-uniform due to subtle temperature unevenness on the substrate surface and the density of surrounding fibers, and the gas that is the source of carbon is consumed by the reaction. As a result, the fiber diameter differs considerably between the inlet and the outlet of the reaction tube, and since production occurs only on the substrate surface, the central part of the reaction tube does not participate in the reaction, resulting in poor yields. However, since there are processes that must be carried out independently, such as dispersing ultrafine particles onto a substrate, reducing them, growing them, and then taking out the fibers, continuous production is impossible, and therefore, there are problems such as poor productivity. Therefore, a method for producing carbon fibers has been proposed in which a mixed gas of a carbon compound gas, an inorganic or organic transition metal compound gas, and a carrier gas is reacted at a high temperature (Japanese Patent Laid-Open Nos. 60-54998, 1983-224816, etc.). [Problems to be solved by the invention] However, Japanese Patent Application Laid-open No. 60-54998, 60-224816
In these methods, since the reaction vessel is also heated, by-products may adhere to the vessel walls, reducing the yield.
Problems such as continuous operation were difficult. In addition, it is not easy to scale up, making it unsuitable for mass production, and requires an electric furnace for heating, resulting in high energy costs. [Means for Solving the Problems] The present invention solves the above problems and provides a method for efficiently manufacturing carbon fibers at low cost. The method for producing carbon fibers of the present invention is a method in which carbon is precipitated into fibers by bringing a carbon compound gas as a raw material into contact with contact particles in a suspended state under laser irradiation. It is characterized by using a laser and using a mixed raw material containing 10 to 50% by volume of ethylene relative to carbon compounds other than ethylene. That is, as a result of intensive studies to solve the conventional problems, the present inventors discovered that under laser irradiation, carbon compound gas and
A method for producing carbon fiber, which is characterized in that carbon fibers are precipitated in the form of fibers by contacting catalyst particles in a suspended state, and a reaction vessel having a reaction zone inside thereof, and an apparatus suitable for carrying out this method. , a laser device that irradiates a laser beam toward the reaction zone, a carrier gas introduction means, a carbon compound gas introduction means, and catalyst particles or catalyst raw materials, which are connected to one side of the reaction vessel with the reaction zone in between. We have developed a carbon fiber production apparatus characterized by comprising a gas introduction means and a carbon fiber collection means connected to the other side of the reaction vessel across the reaction zone, and this invention The present inventors applied for a patent earlier than the applicant (Japanese Patent Application No. 61-234896. Hereinafter referred to as the "prior application"). As a result, they discovered that extremely superior effects can be obtained by using a CO 2 laser as a laser and using a carbon compound containing ethylene as a raw material, and have completed the present invention. The present invention will be explained in more detail below. The carbon compound raw material in the present invention is a mixed raw material of ethylene and all gasifiable carbon compounds other than ethylene. Carbon compounds other than ethylene (hereinafter sometimes simply referred to as "carbon compounds") include CCl 4 , CHCl 3 , CH 2 Cl 2 , CH 3 Cl, CO,
Examples include inorganic compounds such as CS 2 and organic compounds in general. Among these, particularly useful compounds are:
These are aliphatic hydrocarbons and aromatic hydrocarbons. Also,
In addition to these, nitrogen, oxygen, sulfur, fluorine, iodine,
Derivatives containing elements such as phosphorus and arsenic can also be used. Some specific examples of individual compounds include methane (natural gas may also be used), alkane compounds such as ethane, alkene compounds other than ethylene such as butadiene, alkylene compounds such as acetylene, benzene, toluene, and styrene. aryl hydrocarbon compounds such as indene, naphthalene, and phenanthrene; cycloparaffin compounds such as cyclopropane and cyclohexane; cycloolefin compounds such as cyclopentene and cyclohexane; and aliphatic compounds having fused rings such as steroids. Cyclic hydrocarbon compounds, sulfur-containing aliphatic compounds such as methylthiol, methylethyl sulfide, dimethylthioketone, phenylthiol,
Sulfur-containing aromatic compounds such as diphenyl sulfide,
Sulfur-containing heterocyclic compounds such as benzothiophene and thiophene, as well as non-elementary gasoline, Class 4 hazardous materials under the Fire Service Act, Class 1 petroleum, Class 2 petroleum such as kerosene, turpentine, camphor oil, pine oil, and heavy oil. It is also possible to effectively use third-class petroleum oils such as gear oil, cylinder oil, etc. It goes without saying that mixtures of these can also be used. The mixing ratio of such a carbon compound other than ethylene and ethylene is 10 to 50% by volume of ethylene to the carbon compound other than ethylene. If the proportion of ethylene is less than 10%, sufficient energy efficiency improvement effect cannot be obtained by using ethylene.
If it exceeds 50%, the energy will be excessive and the reaction conditions will deteriorate, such as the temperature in the reaction zone becoming too high, making it impossible to expect an improvement in yield. In the present invention, the catalyst includes an inorganic transition metal compound, an inorganic Si inorganic compound, an organic transition metal compound,
Examples include organic compounds of Si. This inorganic transition metal compound is an inorganic transition metal compound that can be vaporized alone, or is soluble in water or at least one kind of water or organic solvent (a carbon raw material compound may be used as the organic solvent). Alternatively, inorganic compounds of transition metals that can be suspended as fine particles are targeted. Transition metals include iron, nickel,
Cobalt, molybdenum, vanadium, palladium, etc. are preferred, and iron is particularly preferred. That is, the CO 2 laser used in the present invention is particularly effective in vibrationally exciting an iron catalyst, and can highly activate the catalyst. The former inorganic transition metal compounds that can be vaporized alone include Fe(NO) 4 , FeCl 3 , Fe(NO) 3 Cl,
Examples include Fe(NO) 2 , Fe(NO) 2 I, and FeF 3 .
In addition to the compounds listed as the former, examples of the latter include Fe(NO 3 ) 2 , FeBr 3 , Fe(HCOO) 3 , C 27 H 42
FeN9O12 , Fe( SO4 ) 3 , Fe(SCN) 3 , Fe (NO) 3
NH 3 , Co(NO) 2 Cl, Ni(NO) Cl, Pd(NO) 2 Cl 2 ,
Representative examples include NiCl 2 and the like. The organic transition metal compounds in the present invention include alkyl metals in which an alkyl group and a metal are bonded, allyl complexes in which an allyl group and a metal are bonded, and π-complexes in which a carbon-carbon double bond or triple bond is bonded to a metal. It is an organic transition metal compound typified by chelate type compounds. In addition, here, the transition metals are:
This refers to scandium, titanium, panadium, chromium, manganese, iron, cobalt, nickel, yttrium, zirconium, niobium, molybdenum, ruthenium, rhodium, palladium, tantalum, tungsten, rhenium, iridium, and platinum. Particularly suitable are those belonging to the periodic table group, among which iron, nickel, and cobalt, with iron being the most suitable for the reasons mentioned above. Furthermore, in the presence of a sulfur-containing carbon compound or an inorganic sulfur compound, an inorganic compound of silicon can also be used. For example, the above-mentioned inorganic metal compounds in which the metal is replaced with Si or silicon carbide can be used. Furthermore, various organosilicon compounds may also be used. The organic silicon compound includes, for convenience, silane and halogen silane in addition to organic compounds having a silicon-carbon bond. Organic compounds with carbon-silicon bonds include organosilanes such as tetramethylsilane and methyltriphenylsilane; organohalogensilanes such as chlorodifluoromethylsilane and promtripropylsilane; methoxytrimethylsilane, trimethylphenoxysilane, etc. organoalkoxysilane; organoacetoxysilane such as diacetoxydimethylsilane, acetoxytripropylsilane; hexaethyldisilane,
Organopolysilanes such as hexaphenyldisilane and octaphenylcyclotetrasilane; organohydrogenosilanes such as dimethylsilane and triphenylsilane; cyclosilanes represented by (SiH 2 ) o ; triphenylsilazane, hexaethyldisilazane, hexa Organosilazane such as phenylcyclotrisilazane, (SiH 2 HN ) Organosilanols such as cyclosilazane diethylsilanediol and triphenylsilanol; Organosilanols such as trimethylsilylacetic acid and trimethylsilylpyropionic acid; Trimethylsilylacetic acid,
Organosilane carboxylic acids such as trimethylsilylpropionic acid and diphenyl silicone diisothiocyanate; trimethyl silicone isocyanate;
Silicon isocyanates such as diphenylsilicon diisocyanate; organosilicon isothiocyanates such as trimethylsilicon isothiocyanate; organosilicon esters such as triethylsilyl cyanide; silthians such as hexamethyldisilthian and telliramethylcyclodisilthian ;
(SiH 2 S) Cyclosylthian represented by o ; organosylmethylenes such as hexamethyldisylmethylene and octamethyltrisylmethylene; organosiloxanes such as hexamethyldisiloxane and hexapropyldisiloxane; It may also be a compound containing other carbon-silicon bonds.
It is also possible to use mixtures of these. Note that, in the present invention, catalyst particles (for example, dried fine powder) that have been generated in advance as fine particles may be introduced into the reaction vessel. The carrier gas in the present invention refers to all gases that are not directly involved in the reaction. Examples include H 2 gas, N 2 gas, NH 3 gas, Ar gas, He
Gas, Kr gas, or a mixture of these gases. Among these, H 2 gas is usually used. Furthermore, a component for enhancing the laser absorption effect may be added to the gas introduced into the container, such as a carrier gas. In this case, the additive components are appropriately selected depending on the wavelength of the laser used, and are used in the present invention.
For CO 2 laser, NH 3 or C 2 H 4 can be added as a laser absorption effect enhancer. The present invention will be described in detail below with reference to preferred embodiments shown in the drawings. FIG. 1 is a schematic cross-sectional view showing an example of an apparatus suitable for carrying out the present invention. Reference numeral 10 is a reaction vessel (in this example, a reaction tube), and one end thereof is filled with CO2.
A CO 2 laser oscillator 12 for irradiating a laser beam is installed, and a laser absorption plate 14 is installed at the other end. Further, on the one end side, a pipe 16 for supplying a compound containing a substance that becomes catalyst particles;
A carrier gas supply pipe 18 and a pipe 20 for supplying a mixed raw material gas of ethylene and carbon compound are connected, and these pipes 16, 18, 2
Flow control devices 16a and 18 are installed in the middle of 0, respectively.
a, 20a are provided. Further, a carbon fiber collector 22 is connected to the other end of the reaction tube 10, and an exhaust gas extraction pipe 24 is connected to the carbon fiber collector 22. In the carbon fiber manufacturing apparatus configured as described above, the compound containing the substance that becomes the catalyst particles introduced into the reaction vessel is excited by the CO 2 laser beam and decomposed, producing catalyst particles such as transition elements or SiC. (The normal particle size is about 0.1 to 10 μm) is produced. Furthermore, the raw carbon compound excited and decomposed by the CO 2 laser beam is deposited on the fine particles, and carbon fibers grow. At this time, the ethylene present in the raw material is excited and generates heat due to absorption of photon energy from the CO 2 laser beam, raising the temperature of the reaction zone to approximately
The temperature is raised to about 1000℃, and the conditions for carbon fiber production are achieved. In the present invention, the temperature of the wall of the reaction vessel in which fine particles are generated and carbon fibers are generated using these as growth points is considerably lower than that of a reaction vessel using a conventional external heating electric furnace. No by-products will be deposited on the wall. Therefore, in the present invention, there is no need to limit the material of the reaction vessel to expensive materials with high corrosion resistance or high heat resistance. Additionally, since it uses a laser beam, it consumes less energy than a general external heating electric furnace, resulting in lower energy costs. However, in the present invention, if necessary, an external heating means such as an external heating type electric furnace may be provided to surround the reaction vessel to heat the vessel wall of the reaction zone. In this case, in order to prevent the product from adhering to the vessel wall, it is preferable to externally heat the vessel so that the vessel wall temperature is less than 600°C, particularly 550°C or less. In the present invention, the size of the catalyst particles or the diameter and length of the carbon fibers can be adjusted by controlling the partial pressure of the raw material gas, residence time, laser intensity, etc. As described above, the reaction order in the reaction vessel is the generation of catalyst fine particles and the growth of carbon fibers, but there is no need to divide the inside of the reaction vessel into a fine particle generation zone and a carbon fiber growth zone.
However, if necessary, a carbon fiber growth zone may be formed by additionally providing a suitable external heating means as described above. The carbon fibers produced in the reaction vessel are introduced into the carbon fiber collector 22 together with a carrier gas. As this collection method, various conventionally known methods such as gravity sedimentation method and electrostatic precipitation method can be employed. Note that the carbon fiber collector 22 also plays a role of cooling the generated carbon fibers. According to the present invention, it is possible to easily produce carbon fibers that usually have a length of about 10 μm to 500 mm and a diameter of about 0.1 to 300 μm. The carrier gas extracted from the carbon fiber collector 22 may be directly introduced into the exhaust treatment means and discharged, but it may also be purified and recirculated for use. In the above apparatus, a laser absorption plate (for example, a water-cooled copper plate) 14 is installed at the end of the reaction tube 10.
If the optical path length is short, a reflector may be placed to lengthen the optical path length of the laser beam. FIG. 2 is a schematic cross-sectional view showing the configuration of another example of a carbon fiber manufacturing apparatus suitable for carrying out the present invention. Reference numeral 30 is a reaction vessel, and in this example, reaction tube 3
2, 34, 36, and 38 are connected and assembled into a rectangular frame shape. A prism 39 is provided at each corner of this rectangle, and a CO 2 laser oscillator 12 is provided at the corner between the reaction tubes 32 and 38.
has been installed. In addition, a window plate is provided at the connection part between the reaction tubes 32 and 38 to allow only the CO 2 laser beam, such as Z o Se, to pass through.
and are blocked. A similar window plate 42 is connected to the reaction tube 34.
and 36. At one end of the reaction tubes 32 and 36, there is a pipe 16 for supplying a compound containing a substance to become catalyst particles, respectively.
A carrier gas supply pipe 18 and a mixed raw material supply pipe 20 of ethylene and carbon compound are connected to each other, and flow rate control devices 16a, 18a, and 20a are provided in the middle of these pipes. Furthermore, carbon fiber collectors 22a and 22b are connected to the end of the reaction tube 34 on the reaction tube 36 side and the end of the reaction tube 38 on the reaction tube 32 side, respectively.
An exhaust gas outlet 24 is connected to a and b. In the apparatus of FIG. 2 configured in this way,
The gas introduced from the pipes 16, 18 and 20 reacts in the reaction tubes 32 and 34 to generate carbon fibers,
This carbon fiber is collected by the collector 22a. Furthermore, the carbon fibers generated in the reaction tubes 36 and 38 are
Similarly, it is collected by the collector 22b. In the device shown in Fig. 2, the optical path length of the CO 2 laser beam is large;
Carbon fiber can be manufactured efficiently. In the above embodiment, the reaction tubes are connected in a rectangular shape to constitute the reaction vessel, but this may be in other shapes such as pentagonal or hexagonal. Furthermore, various connection methods may be employed, such as a connection method in which the reaction tubes are reciprocated in a zigzag manner, and a multi-type connection method in which reaction tubes are arranged in parallel. FIG. 3 is a perspective view showing a different configuration example of a carbon fiber manufacturing apparatus suitable for carrying out the present invention. This device includes two flat plates 40 and 42 and a laser reflecting plate 4.
4, 46 and the laser absorption plate 48 constitute a reaction vessel 50. In this reaction vessel 50, a mixed gas of ethylene and a carbon compound, a carrier gas, and a compound gas containing a substance that will become catalyst particles are introduced from the gas introduction side 50a, and the CO 2 laser oscillator 12 is directed toward the laser reflection plate 44. It is emitting laser light. This CO 2 laser is reflected multiple times between the reflection plates 44 and 46, and eventually reaches the laser absorption plate 48.
However, during this process, the above gas is excited and carbon fibers are produced. The generated carbon fibers are discharged from the outlet side 50b of the reaction vessel 50 together with the carrier gas and the remaining raw material gas, and the carbon fibers are collected by an appropriate collection means. Note that the CO 2 laser oscillator 12 may be moved in the longitudinal direction of the reaction container 50 so as to swing its head. In this way, the entire inside of the reaction vessel 50 can be irradiated with the CO 2 laser beam, and the carbon fiber production reaction is further promoted. Further, instead of making the CO 2 laser oscillator 12 swing, a CO 2 laser oscillator 12 that emits a laser beam in a diffusing direction may be used.
In this case, it is necessary to make all parts of the reaction vessel 50 other than the laser absorption plate installation part a mirror surface to reflect the laser beam. Further, by employing a curved mirror as the laser reflecting plate 44, the laser beam may be emitted toward the laser reflecting plate 44. Even in this case, the inner surface of the reaction vessel other than the laser absorption plate needs to have a mirror surface. [Effect] The CO 2 laser has a particularly excellent effect of efficiently vibrationally exciting a catalyst such as an iron catalyst to develop high activity. On the other hand, since ethylene has an absorption band in the approximately 10.6 μm wavelength range of the CO 2 laser, by mixing a specific proportion of ethylene into the raw material, heat generation occurs due to photon energy absorption of ethylene, which can easily lower the temperature of the reaction zone. It is possible to set the carbon fiber generation temperature condition to about 1000℃. Therefore, according to the method of the present invention, it is possible to improve energy efficiency, lower the heating temperature, and improve the yield. [Example] Hereinafter, preferred manufacturing examples will be described. Example 1 In the apparatus shown in FIG. 1, carbon fibers were manufactured under the following conditions. Laser: CO 2 laser (10.591 μm) Mixed raw materials: Methane: Thielene = 100:30 (volume ratio) Compound containing the substance that becomes catalyst particles: FeCl 3 aqueous solution Carrier gas: H 2 pressure Pressure: Normal pressure Residence time: 1 minute Raw material concentration: 5 vol% relative to H 2 Reactor: 20 mm ID x 450 mm L (made of quartz) The results are shown in Table 1. Examples 2 to 4, Comparative Examples 1 to 3 Carbon fibers were produced in the same manner as in Example 1, except that the volume ratio of methane and ethylene in the mixed raw materials was set to the values shown in Table 1. The results are shown in Table 1. As is clear from Table 1, according to the method of the present invention, carbon fibers can be produced in high yield. In addition, in Examples 1 to 4, no deposits were observed on the vessel wall.
【表】
［発明の効果］
以上の通り、本発明はCO2レーザによる触媒の
活性化及び原料炭素化合物の励起、分解、更に
CO2レーザの波長域に吸収帯を持つエチレンの光
子エネルギー吸収による発熱を利用して気相法に
より炭素繊維を製造するものであり、
エネルギー消費が少なく、製造コストが廉価
である。
反応容器の内壁面は低温であり、その材質も
廉価な材質のもので足りる。
反応容器内面に副生物が付着しにくく、連続
運転及び大型反応容器の稼動に好適である。
反応容器内の圧力、各ガスの分圧、滞留時
間、レーザ強度等を調節することにより得られ
る炭素繊維の品質を容易に制御することができ
る。
大量生産、スケールアツプが容易である。
触媒の活性化効率、エチレンによる発熱効率
が高いため、収率、反応速度、エネルギー効率
が著しく高い。
等の優れた効果が奏される。[Table] [Effects of the Invention] As described above, the present invention can activate a catalyst using a CO 2 laser, excite and decompose a raw material carbon compound, and further
Carbon fiber is produced by a vapor phase method using the heat generated by photon energy absorption of ethylene, which has an absorption band in the CO 2 laser wavelength range, resulting in low energy consumption and low manufacturing costs. The inner wall surface of the reaction vessel is at a low temperature, and its material can be made of an inexpensive material. It is difficult for by-products to adhere to the inner surface of the reaction vessel, making it suitable for continuous operation and operation of large reaction vessels. The quality of the carbon fiber obtained can be easily controlled by adjusting the pressure inside the reaction vessel, the partial pressure of each gas, residence time, laser intensity, etc. Mass production and scale-up are easy. Because the activation efficiency of the catalyst and the heat generation efficiency of ethylene are high, the yield, reaction rate, and energy efficiency are extremely high. Excellent effects such as these can be achieved.
第１図、第２図及び第３図はそれぞれ本発明の
実施に好適な炭素繊維製造装置の構成説明図であ
る。
１０……反応容器、１２……レーザ発振器、１
６……触媒供給管、１８……キヤリアガス供給
管、２０……炭素化合物供給管、２２，２２ａ，
２２ｂ……炭素繊維捕集器。
FIG. 1, FIG. 2, and FIG. 3 are respectively explanatory diagrams of the configuration of a carbon fiber manufacturing apparatus suitable for carrying out the present invention. 10... Reaction container, 12... Laser oscillator, 1
6... Catalyst supply pipe, 18... Carrier gas supply pipe, 20... Carbon compound supply pipe, 22, 22a,
22b...Carbon fiber collector.
Claims (1)
ガスと、浮遊状態にある触媒粒子とを接触させて
炭素を繊維状に析出させる方法であつて、レーザ
としてCO2レーザを用いると共に、原料として、
エチレン以外の炭素化合物に対して、エチレンを
10〜50体積％含む混合原料を用いることを特徴と
する炭素繊維の製造方法。1 A method of depositing carbon in the form of fibers by contacting a carbon compound gas as a raw material with suspended catalyst particles under laser irradiation, using a CO 2 laser as the laser, and using as a raw material,
For carbon compounds other than ethylene, ethylene
A method for producing carbon fiber, characterized by using a mixed raw material containing 10 to 50% by volume.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62243292A JPS6485320A (en) | 1987-09-28 | 1987-09-28 | Production of carbon fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62243292A JPS6485320A (en) | 1987-09-28 | 1987-09-28 | Production of carbon fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6485320A JPS6485320A (en) | 1989-03-30 |
| JPH0440450B2 true JPH0440450B2 (en) | 1992-07-03 |
Family
ID=17101671
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62243292A Granted JPS6485320A (en) | 1987-09-28 | 1987-09-28 | Production of carbon fiber |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6485320A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2021516160A (en) * | 2018-05-07 | 2021-07-01 | フロニウス・インテルナツィオナール・ゲゼルシャフト・ミット・ベシュレンクテル・ハフツングＦｒｏｎｉｕｓ Ｉｎｔｅｒｎａｔｉｏｎａｌ Ｇｍｂｈ | A method for automatically determining the optimum welding parameters for performing work piece welding |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI466604B (en) * | 2008-12-08 | 2014-12-21 | Unimicron Technology Corp | Wiring board and fabrication process thereof |
-
1987
- 1987-09-28 JP JP62243292A patent/JPS6485320A/en active Granted
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2021516160A (en) * | 2018-05-07 | 2021-07-01 | フロニウス・インテルナツィオナール・ゲゼルシャフト・ミット・ベシュレンクテル・ハフツングＦｒｏｎｉｕｓ Ｉｎｔｅｒｎａｔｉｏｎａｌ Ｇｍｂｈ | A method for automatically determining the optimum welding parameters for performing work piece welding |
| US11815877B2 (en) | 2018-05-07 | 2023-11-14 | Fronius International Gmbh | Method for automatically determining optimum welding parameters for carrying out a weld on a workpiece |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6485320A (en) | 1989-03-30 |
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