Reclamation of carbon fibers and added-value gases in a pyrolysisbased composites recycling process

Reclama ion o ca bon ibe s and added- alue gases in a py olysis-based composi es ecycling p ocess A. Lopez-U ionaba enechea1*, N. Gas elu1, E. Acha1, B.M. Caballe o1, A. O ue2, A. Jiménez- Suá ez3, S.G. P olongo3, I. de Ma co1 1 Chemical and En i onmen al Depa men , Facul y o Enginee ing o Bilbao. Uni e si y o he Basque Coun y (UPV/EHU). Plaza Ingenie o To es Que edo 1, 48013 Bilbao (Spain). 2 Chemical and En i onmen al Depa men , Facul y o Enginee ing o Gipuzkoa. Uni e si y o he Basque Coun y (UPV/EHU). Plaza Eu opa 1, 20018 Donos ia-San Sebas ian (Spain). 3 Ma e ials Science and Enginee ing A ea, ESCET. Uni e si y Rey Juan Ca los. C/Tulipán s/n, Mós oles, Mad id (Spain) Co esponding au ho in o ma ion: This is he accep ed manusc ip o he a icle ha appea ed in inal o m in Jou nal o Cleane P oduc ion 273 : (2020) // A icle ID 123173, which has been published in inal o m a h ps://doi.o g/10.1016/ j.jclep o.2020.123173. © 2020 Else ie unde CC BY-NC-ND license (h p://c ea i ecommons.o g/licenses/by- nc-nd/4.0/) 1 Abs ac 1 Ca bon ibe s eclama ion om was e composi es by py olysis is de eloping as . Py olysis 2 allows he eclama ion o he ibe s by he mal decomposi ion o he polyme ic esin, bu he 3 ma e ial alue o hese esins is no ye eco e ed. In his esea ch wo k, he possibili y o 4 ob aining high- alue gaseous ac ions by ea ing he apo s gene a ed in he decomposi ion 5 o a poly(benzoxazine) con aining ca bon ibe was e composi e has been s udied. The 6 expe imen s ha e been ca ied ou in a lab-scale acili y consis ing o wo eac o s in se ies. In 7 he i s eac o , he py olysis o he was e is ca ied ou a 500 °C, while in he second eac o 8 he apo s coming om he i s eac o a e ea ed a 900 °C. Such ea men enables o iple 9 he amoun o gas in compa ison o con en ional py olysis. Besides, his gas con ains 56% by 10 olume o H2, which means he eco e y o app oxima ely 60% o he hyd ogen con ained in he 11 esin. On he o he hand, clean ca bon ibe s wi h mechanical p ope ies wi hin comme cial 12 alues ha e been also ob ained. 13 14 Keywo ds: ca bon ibe , py olysis, ca bon composi es, ecycling, poly(benzoxazine), seconda y 15 aw ma e ials. 16 17 Wo dcoun : 7915 18 19 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 2 1. In oduc ion 20 21 Ca bon ibe (CF) is a e y low-densi y ma e ial wi h excellen mechanical, elec ical and he mal 22 p ope ies, which is almos exclusi ely used as ein o cemen o plas ic ma ix composi e 23 ma e ials, called ca bon ibe ein o ced plas ics/polyme s (CFRP) (Gio gini e al., 2015). Behind 24 he gene ic de ini ion o CFRP, he e is a wide a ie y o p oduc s co e ing la ge anges o 25 physical-chemical p ope ies. This is because such p ope ies depend undamen ally on he 26 quali y o he ibe s - which can be manu ac u ed almos o measu e acco ding o he needs in 27 se ice - and he quan i y, leng h and o ien a ion o he ibe s wi hin he plas ic ma ix - bo h 28 leng h and alignmen inc easing he ein o cemen capaci y o he ibe s - (Newcomb, 2016; 29 William D. Callis e J ., 2014). This ci cums ance gi es CFRP a e sa ili y ha explains hei 30 massi e and g owing indus ial and u ban use (Holmes, 2017a; Liu e al., 2019; Vo Dong e al., 31 2019). 32 33 Howe e , CF p oduc ion is a p ocess wi h high en i onmen al and ene gy impac . 96% o CF is 34 p oduced om poly(ac yloni ile) (PAN) ibe s (Newcomb, 2016). PAN is ob ained by 35 polyme iza ion o ac yloni ile, which in u n is he p oduc o he eac ion be ween p opylene 36 and ammonia, bo h o hem o iginally coming om oil (Naq i e al., 2018). PAN ibe s a e 37 ca bonized in a empe a u e ange be ween 1000 °C o 3000 °C, depending on he speci ic 38 p ope ies desi ed o he CF. Finally, CF a e condi ioned h ough su ace ea men s (Naq i e 39 al., 2018; Newcomb, 2016). In summa y, CF is a ossil p oduc ha is manu ac u ed h ough a 40 mul i-s age p ocess whe e e y high empe a u es, sol en s, inishing oils and su ace ea men 41 esins a e equi ed. Addi ionally, a mosphe ic emissions o oxic compounds such as HCN, NH3 42 o NOx om u naces and eac o s a e p oduced (Le eu e e al., 2017; Vo Dong e al., 2018). 43 44 One way o educe he impac o he g owing CF p oduc ion is o eco e hem om esidual 45 CFRP and e-manu ac u e composi e ma e ials wi h he eclaimed ibe s (He mansson e al., 46 2019). The e is s ill much o be de eloped in his ield, as al hough se e al me hods o CF 47 eco e y ha e been in es iga ed, land ill and incine a ion a e oday he wo mos common ways 48 o managing CFRP was e (Liu e al., 2017; Vo Dong e al., 2018; Yang e al., 2012). In o de o 49 eco e he CF om a composi e ma e ial i is necessa y o emo e he polyme ic esin whe e 50 hey a e embedded. This can be done by dissolu ion (chemical me hods) and by decomposi ion 51 ( he mal me hods) (Pimen a and Pinho, 2011; Rybicka e al., 2016). Recen ly published 52 economic, en i onmen al and human heal h impac assessmen s compa ing hese al e na i es 53 poin o he la e as he op ion wi h lowes impac , pa icula ly when he he mal me hod is 54 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 3 py olysis (Khalil, 2018; Vo Dong e al., 2018). Consequen ly, py olysis is he mos ma u e 55 echnology, wi h he highes TRL and he la ges numbe o indus ial implemen a ions, despi e 56 he ac ha chemicals a e no eco e ed om he esin (i is bu ned) while dissolu ion me hods 57 a e heo e ically capable o eco e ing he ibe s and some monome s, mainly phenol and 58 de i a i es (Kim e al., 2019; La Rosa e al., 2016). 59 60 Py olysis is hea ing in he absence o oxygen. In he case o CFRP was e, he inal empe a u e is 61 usually be ween 400 and 600 °C, a which mos esins a e b oken down bu do no CF (Meng e 62 al., 2018; Meye e al., 2009; Wong e al., 2010). The decomposi ion o he polyme ic esin 63 p oduces gases, apo s (liquids a oom empe a u e) and a ca bonaceous p oduc (cha ) ha 64 o ms a ligh laye co e ing he ca bon ibe s. This laye o cha can p e en he p ope adhesion 65 o he eclaimed ibe s wi h new esins a he ime o euse, so i is necessa y a pos - ea men 66 in he p esence o ai o elimina e i (Onwudili e al., 2016). This pos - ea men mus be 67 con olled (no e y high empe a u e and no e y long ime) in o de o a oid he deg ada ion 68 o he ibe s by combus ion (López e al., 2013; Nahil and Williams, 2011). Acco ding o 69 specialized li e a u e, his p ocess does no signi ican ly damage he CF, which e ain hei 70 ensile modulus o elas ici y and 90% o hei ensile s eng h (Holmes, 2018; Pimen a and Pinho, 71 2014). 72 73 Howe e , he ecycling o CFRP was e by py olysis has no been launched de ini i ely. The 74 s udies indica e ha i is s ill necessa y o make he ecycling p ocess mo e p o i able. The e a e 75 wo a eas wi h g ea po en ial o imp o emen : (1) ob aining longe ibe s and de eloping 76 echniques o aligning sho and long ecycled ca bon ibe s (Holmes, 2018, 2017b; Meng e al., 77 2018) and (2) ma e ial eco e y om polyme ic esins (Cousins e al., 2019; Vo Dong e al., 2018). 78 The la e is no an easy ask since CFRP py olysis liquids a e complex mix u es o ni ogenous, 79 oxygena ed and sulphu o ganic compounds, o en mixed wi h wa e . On he o he hand, he 80 gases, composed o ca bon monoxide and dioxide, hyd ogen and ligh hyd oca bons, a e 81 gene a ed in low quan i y (López e al., 2013; Nahil and Williams, 2011; Yang e al., 2015). 82 83 The gases could be used as an al e na i e uel, bu he bene i ob ained om hem would no 84 compensa e o he p oblem gene a ed by he liquid p oduc , whose indus ial use is unlikely, 85 wi h he esul ha i would be classi ied as a haza dous was e. The e o e, i is e iden ha a 86 ea men is necessa y o y o imp o e he composi ion o liquids and/o o elimina e hem in 87 a o o he gaseous ac ion. Howe e , as a as we a e conce ned, he e is no e idence om 88 any esea ch g oup ha has in es iga ed his issue o da e. The au ho s o his a icle ha e 89 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 4 de eloped a me hod based on he he mo-ca aly ic ea men o such gases and apo s be o e 90 condensa ion (Gas elu e al., 2019, 2018). This me hod a oids he emission o gaseous p oduc s 91 om esin combus ion and eco e s added- alue gases. The objec i e o he p esen pape is o 92 de e mine he maximum pe o mance o he ea men in he absence o ca alys , by s udying 93 he in luence o he ille used ea men eac o . 94 95 2. Ma e ials and me hods 96 97 2.1. CFRP was e 98 The CFRP was e a e p e-p eg pieces om ae onau ical indus y composed o a 99 poly(benzoxazine) ype polyme ic esin and To ay T300/3k ca bon ibe s ab ic in he o m o 100 plain wea e. Table 1 shows some chemical p ope ies o he CFRP sample. A deepe discussion 101 o hese p ope ies and he he mal beha io o his sample has been epo ed elsewhe e 102 (Gas elu e al., 2018). 103 104 Table 1. Fibe con en , p oxima e analysis and elemen al analysis o he was e CFRP (w .%). 105 Fibe con en 61.0 P oxima e analysis Mois u e 0.5 Vola iles 28.4 Fixed ca bon1 71.0 Ash 0.1 Elemen al analysis C 86.2 H 2.2 N 4.8 S 1.3 Cl u.d.l.2 O he s3 4.9 1 By di e ence 106 2 Unde de ec ion le el (<0.1 w .%) 107 3 O he s = 100-(C+H+N+S+Mois u e+Ash) 108 109 2.2. Lab-scale ins alla ion o ca bon ibe eclama ion 110 The expe imen s we e ca ied ou in a lab-scale ins alla ion consis ing o wo eac o s connec ed 111 in se ies and a sec ion o condensa ion o liquid p oduc s and cleaning o gases (see Figu e 1). 112 The i s eac o (3) is a non-s i ed ank eac o 15 cm in diame e and 21 cm in heigh . The 113 second eac o (6) is a ixed bed ubula eac o 2.5 cm in diame e and 50 cm in leng h. The wo 114 eac o s a e made o 316 s ainless s eel and a e ex e nally hea ed by elec ic u naces. The 115 ou pu o he second eac o (9) is connec ed o h ee condense s (11, 12, 13) and an ac i a ed 116 ca bon column (Pan eac Ac i a ed Ca bon No. 1 QDP). The non-condensable p oduc s pass 117 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 5 h ough he ac i a ed ca bon column (14) and hen hey a e collec ed in gas sampling bags (16, 118 17). 119 120 121 122 1 Ro ame e 11 Condense 1 2 Py olysis / oxida ion eac o 12 Condense 2 3 Py olysis / oxida ion u nace 13 Condense 3 4 Fu nace he mocouple 14 Ac i a ed ca bon column 5 Reac o he mocouple 15 T al e 6 Tubula eac o 16 Gas bag 1 7 Tubula u nace 17 Gas bag 2 8 Tubula eac o he mocouple 18 Tubula u nace empe a u e-con ol 9 Vapo and gas ou le 19 Py olysis / oxida ion u nace empe a u e-con ol 10 Solid bed ma e ial 20 Compu e Figu e 1. Flowshee o he py olysis ins alla ion. 123 124 In a ypical expe imen , 100 g o CFRP was e (cu in o 20 x 2 cm shee s) is in oduced in o he 125 i s eac o , which is hea ed up a 3 °C min-1 o 500 °C o 30 minu es and is ed wi h a 1 L min- 126 1 low a e o N2. The gene a ed gases and apo s pass h ough he ubula eac o , hea ed a 127 900 °C, whe e a second he mal c acking akes place. This eac o is illed wi h a solid bed 128 ma e ial in o de o imp o e luid dynamics and a oid empe a u e g adien s. Once he py olysis 129 s age is comple ed, he eed gas is changed o syn he ic ai in o de o accomplish an oxida ion 130 s age a 500 °C o 45 minu es, using an ai low a e o 1.5 L min-1. This pape p esen s he esul s 131 o i e di e en expe imen s. The i s one (E1) is a con en ional py olysis es , wi hou 132 ea men o gases and apo s. In he o he ou expe imen s (E2-E5) such ea men does occu 133 and he in luence o he cha ac e is ics o he solid bed placed wi hin he ubula eac o is 134 s udied. 135 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 6 2.3. Ma e ials employed in he solid bed 136 Th ee ypes o ma e ials we e used as ille s o he ubula eac o . On he one hand, silicon 137 ca bide (CSi) p o ided by Na a osic S.A., wi h wo di e en pa icle size dis ibu ions, 1.5 mm 138 < x < 2 mm and 0.5 mm < x < 1 mm. CSi is a e ac o y ma e ial p esen ing good he mal 139 conduc i i y and high s abili y in he condi ions o he apo s ea men (Dey e al., 2014). I is 140 widely used as solid bed in chemical eac o s on a labo a o y scale, since i imp o es luid 141 dynamics and hea anspo h oughou hem (O ega e al., 2018; Song e al., 2018; Tillmann 142 e al., 2018). 143 144 The second solid bed ma e ial was made om de ec i e b icks o composi ion 50-65% Al2O3, 30- 145 40% SiO2, 1-2% Fe2O3, 0.5-1.5% Na2O+K2O in weigh , p o ided by Be oa S.L. O iginally b ick 146 shaped, hey we e g ound o 1.5 < x < 2 mm pa icle size. This is a highly e ac o y ma e ial 147 (Sege Cone num. 37), so i s unc ion was expec ed o be equi alen o ha o CSi bu a a much 148 lowe cos ( hey a e was e b icks). In addi ion, he p esence o alkali me al oxides and i on oxide 149 could ha e some ca aly ic e ec ha could be bene icial o he p ocess. 150 151 Finally, a me allu gical coke o low ola ile con en p o ided by Be esa Zinc Ase S.A. was also 152 employed as solid bed ma e ial. O iginally i was in he o m o small b ique es, so i was g ound 153 o 1.5 < x < 2 mm pa icle size. The objec i e o using a ca bonaceous subs ance as solid bed is 154 o obse e i s ca aly ic ac ion capaci y in con ac wi h CFRP decomposi ion subs ances, since 155 ca bonaceous ma e ials a e widely es ed subs ances o he ea men o oxygena ed 156 subs ances and a s (Elkasabi e al., 2017; Ra enni e al., 2018). In his speci ic case, a 157 me allu gical coke has been selec ed because i is a “low-in- ola iles” ma e ial and he e o e 158 ela i ely s able a he empe a u e o he ea men ca ied ou a he ubula eac o (900 °C). 159 160 Table 2 shows he mos ep esen a i e ex u al pa ame e s o he ille s. In gene al, hey show 161 a e y low su ace a ea, so hey can p ac ically be conside ed non-po ous, especially CSi. As 162 ega ds he o he analyses ca ied ou on hese ma e ials, he acidi y analyses do no show any 163 app eciable acidic cha ac e is ics, so ha nei he coke no e ac o y can be conside ed as an 164 acid ma e ial. In addi ion, he e ac o y does no exhibi educible species wi h H2 (TPR) o 165 in e ac ion wi h CO, so i can be conside ed a subs ance wi h s able me al oxides. The da a 166 ob ained in hese analyses a e no p esen ed in he manusc ip because hey lack ele an 167 in o ma ion, bu some analysis esul s a e included in he appendix o he a icle. 168 169 170 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 7 Table 2. Tex u al p ope ies o he ma e ials employed in he solid bed. 171 CSi Coke Re ac o y Su ace a ea (m2 g-1) 0.085 1.18 0.28 Po e olume (cm3 g-1) 4.18·10-4 3.48·10-3 6.15·10-4 Po e diame e (Å) 34.8 33.9 55.8 172 2.4. Analy ical echniques 173 The ca bon ibe con en o he CFRP was de e mined using he ASTM D3171 (P ocedu e B), 174 which consis s o he chemical dissolu ion o he esin in a mix u e o sul u ic acid and hyd ogen 175 pe oxide. The ul ima e analysis was de e mined wi h he LECO T ueSpec CHN and LECO 176 T ueSpec S elemen al analyze s espec i ely. Addi ionally, he p esence o elemen al chlo ine 177 was examined by applying Me hod 5050 o he US En i onmen al P o ec ion Agency (EPA). This 178 me hod is based on he combus ion o he sample in a calo ime ic pump (LECO AC-500) and 179 he subsequen abso p ion o he combus ion gases in a basic solu ion, which is analyzed by ion 180 ch oma og aphy (Dionex ICS 3000, equipped wi h conduc i i y and ampe ome ic de ec o s). 181 The p oxima e analysis was pe o med wi h he LECO TGA-500 he mobalance, which ollows 182 he ASTM D3173-85 and D3174-82 s anda ds. 183 184 The ex u al p ope ies o he solid bed ma e ials was de e mined using he N2 adso p ion- 185 deso p ion me hod in an Au oso b 1C-TCD. The samples we e p e iously degassed a 300 °C o 186 12 h. The su ace a ea was calcula ed using he B unaue -Emme -Telle (BET) me hod, while 187 he po e dis ibu ion was calcula ed using he Ba e -Joyne -Halenda (BJH) me hod. The acidi y 188 o he e ac o y ma e ial was analyzed by empe a u e p og ammed deso p ion o ammonia 189 (NH3-TPD) while he educible me als we e sough by empe a u e-p og ammed educ ion 190 (TPR), bo h o hem by using he Mic ome i ics® Au oChem II equipmen . This equipmen was 191 also used o analyze he p esence o ca aly ically ac i e me als on he su ace o e ac o y by 192 chemiso p ion wi h CO. 193 194 The py olysis solids we e cha ac e ized h ough ul ima e and p oxima e analysis, ollowing he 195 p ocedu e used wi h he CFRP sample. The composi ion o he liquid p oduc s was de e mined 196 using a gas ch oma og aph (GC, Agilen 6890) coupled o a mass spec ome e (MS, Agilen 197 5973), conside ing as iden i ied only such chemicals p o iding an iden i ica ion quali y 198 pa ame e g ea e han 85%. The gaseous p oduc s we e analyzed in a gas ch oma og aph 199 (Agilen 7890A) wi h he mal conduc i i y and lame ioniza ion de ec o s (TCD and FID, 200 espec i ely). This ch oma og aph is calib a ed o de e mine he composi ion o he so-called 201 " e ine y mix u e", which includes H2, CO, CO2, CH4, C2, C3, C4, C5 and C6. The highe hea ing 202 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 8 alue (HHV) o he gases was calcula ed om he HHV o he pu e compounds ha a e pa o 203 hei composi ion. 204 205 The eclaimed CF we e also subjec ed o ul ima e and p oxima e analyses acco ding o he 206 p ocedu e men ioned abo e. The mo phological cha ac e is ics we e e alua ed by scanning 207 elec on mic oscopy (SEM), wi h ene gy-dispe si e X- ay spec oscopy (EDX) o he 208 de e mina ion o he su ace composi ion, using he Hi achi S-2400N mic oscope. Mechanical 209 p ope ies we e measu ed by means o Minima 2000 es e (Rheome ic Scien i ic) equipped 210 wi h a load cell o 200 N a a es ing speed o 1 mm min-1. CF we e moun ed and glued on a 211 pape ab ha was placed in he g ips. Then, he middle po ion o he pape s was cu , so ha 212 only he ca bon ibe ca ied he load (Luo and Ne a ali, 2001). 10 mm clamping leng h was 213 used and a leas 10 specimens we e es ed, being he a e age alues epo ed. 214 215 3. Resul s and discussion 216 217 3.1. Py olysis s age 218 Table 3 shows he py olysis yields and he composi ion o he gases and liquids ob ained in he 219 i e es s. These py olysis yields a e he a e age alue o a leas wo iden ical expe imen s 220 whe e he e was no a a ia ion g ea e han 3% in he yields hemsel es. These yields a e 221 quan i ied as ollows: (1) solids yield co esponds o he emaining sample in he eac o a e 222 he py olysis s age, (2) he yield o o al condensa es is de e mined by he di e ence in weigh 223 o he pipes and condense s be o e and a e he expe imen , and (3) he gas yield is calcula ed 224 by di e ence. The "collec ed liquids" is he amoun o liquids in he condense s, which is 225 dis inguished wi hin he o al condensa es yield wi h he in en ion o gi ing ep esen a i e 226 in o ma ion o he p ocess pa ame e s and no so much o he geome y o he ins alla ion, 227 which can ha e much in luence on he amoun o condensa es gene a ed in he pipes and o he 228 elemen s. These collec ed liquids ha e been used o de e mine he composi ion o condensa es 229 and he p opo ions o aqueous phase and o ganic phase. The gas composi ion shown in he 230 able is d y and ee o N2. 231 232 233 234 235 236 237 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 15 398 Figu e 3. SEM images o eclaimed ca bon ibe s. 399 400 Ene gy-dispe si e X- ay spec oscopy (EDX) has been used o de e mine he su ace composi ion 401 o he CF, as well as ha o he pa icles seen on SEM mic og aphs. The esul s a e p esen ed in 402 Figu es 4 and 5. Fi s ly, one smoo h a ea has been analyzed, ha is, he su ace o he ibe s 403 (Figu e 4). The spec og am shows ha he only elemen de ec ed on ha su ace is ca bon, 404 which could indica e ha i is he su ace o he clean ibe , and he e o e would indica e a good 405 eclama ion o he ma e ial. P e ious esea ch on oxida i e ea men s o CFRP was e has also 406 shown small amoun s o oxygen on he su ace o he eclaimed ibe s (Yip e al., 2002). In 407 gene al, he amoun o su ace oxygen inc eases wi h he agg essi eness o he oxida ion 408 p ocess (long ime, high empe a u e), so he absence o su ace oxygen could be indica i e o 409 con olled and no excessi e oxida ion. 410 411 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 16 412 Figu e 4. Ca bon ibe s su ace composi ion analysis. 413 414 Figu e 5 shows he spec og ams o wo pa icles deposi ed on he ibe s. I can be seen ha he 415 main elemen o hei composi ion is again ca bon, ollowed by oxygen, sodium and sulphu . 416 The p esence o oxygen and sulphu may indica e some aces o he polyme ic esin, while he 417 appea ance o sodium on he su ace is a p io i qui e su p ising. Howe e , he e is a p eceden 418 epo ing he p esence o sodium in eclaimed ibe s om CFRP. In ha wo k, he exis ence o 419 sodium was a ibu ed o he manu ac u ing p ocess o he ca bon ibe s (Jiang e al., 2008). 420 421 422 423 Figu e 5. Composi ion o su ace pa icles. 424 425 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 17 The mechanical cha ac e iza ion o he eclaimed ibe s is p esen ed in Table 5. The pa ame e s 426 measu ed a e he usual ones in mechanical cha ac e iza ion o his ma e ial, ha is, ensile 427 s eng h, ensile modulus and elonga ion a b eak. The alues o he same pa ame e s o some 428 comme cial CF ha e been also included in his able, ob ained om comme cial ca alogues and 429 a ailable echnical da a shee s. I can be seen ha he eco e ed ibe s ha e a conside ably 430 lowe ensile modulus han he comme cial ibe s o he TORAYCA and he YS se ies o GRANOC, 431 all o hem common in s uc u al ae onau ical applica ions. Howe e , he ensile s eng h, 432 al hough also lowe , is in he o de o magni ude o he TORAYCA T300 and GRANOC YS-90A- 433 30S ibe s. 434 435 Table 5. Mechanical p ope ies o eclaimed ca bon ibe s and some comme cial ca bon ibe s. 436 437 The CFRP was e used in his wo k has been gene a ed in p oduc ion asks o he ae onau ical 438 indus y, bu bo h i s speci ic applica ion and he p ope ies o he o iginal ibe s a e unknown, 439 so i is no possible o de e mine he deg ee o de e io a ion ha he mechanical p ope ies o 440 he ibe s may ha e su e ed du ing he ecycling p ocess. Howe e , he conse a ion o he 441 mechanical p ope ies o CF eco e ed by py olysis is a ac ha is p o en in he scien i ic 442 li e a u e ela ed o CFRP ecycling, as discussed in he in oduc ion o his a icle (Naq i e al., 443 2018; Pimen a and Pinho, 2014, 2011). The low alues obse ed in his s udy may be due o he 444 speci ic cha ac e is ics o he eac o used o o he unce ain y and dispe sion o he esul s 445 ob ained in he analysis o such small diame e ibe s, as some esea che s ha e poin ed ou 446 (Gille e al., 2015). 447 448 In any case, he elonga ion a b eak and ensile modulus o he eclaimed ibe s a e equi alen 449 o hose o he GRANOC XN se ies ibe s, which a e classi ied as low modulus and high elonga ion 450 ibe s. In addi ion, hei ensile s eng h is signi ican ly highe han he s eng h o hese 451 comme cial ibe s. The e o e, i is clea ha he CF eco e ed in his wo k can ha e alue and 452 Tensile s eng h (MPa) Tensile modulus (GPa) Elonga ion a b eak (%) Reclaimed ibe s 2678 ± 700 96 ± 20 2.6 ± 0.8 TORAYCA T300 3530 230 1.5 TORAYCA T800S 5880 294 2.0 GRANOC YS-90A-30S 3530 880 0.3 GRANOC XN-10-30-S 1700 110 1.6 GRANOC XN-05-30-S 1100 54 2.0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 18 comme cial applica ions and compe e wi h i gin ca bon ibe s o ossil o igin. These esul s 453 demons a e he compe i i eness o eclaimed ca bon ibe s as seconda y aw ma e ials. 454 455 4. Conclusion 456 457 The main conclusions ha can be d awn om he wo k p esen ed in his a icle a e he 458 ollowing: 459 460 - Py olysis and oxida ion o poly(benzoxazine) ype CFRP was e allows he eco e y o ca bon 461 ibe s ha p esen mos ly clean su aces and mechanical p ope ies simila o some comme cial 462 i gin ca bon ibe s. 463 - The cooling and condensa ion o he apo s om he py olysis s age gene a es a liquid and a 464 gaseous ac ion. The liquid ac ion is composed o an aqueous and an o ganic phase, bo h o 465 which a e o low alue due o hei complex composi ion based on ni ogenous and oxygena ed 466 a oma ic compounds. The gaseous ac ion is composed o CH4 and CO2, i has low calo i ic alue 467 and is gene a ed in small quan i ies. 468 - I he apo s a e ea ed a high empe a u e (900 °C) in a CSi- illed eac o , he amoun o 469 liquids gene a ed is signi ican ly educed, inc easing he p opo ion o gases o mo e han 470 double. These gases imp o e hei composi ion signi ican ly, en iching hemsel es wi h H2 and 471 educing hei CO2 con en , which doubles hei calo i ic alue. 472 - I has been p o en ha he ma e ial used as solid bed in he ubula eac o has an app eciable 473 in luence. The bes esul s ha e been ob ained by using a esidual e ac o y ma e ial, hanks o 474 which he p o i abili y o he p ocess inc eases conside ably. This is why: (1) i is a was e ma e ial 475 and (2) i gene a es a H2 p opo ion highe han 50% by olume in he gases, which enables he 476 sepa a ion o H2 as a pu e compound, p esen ing a wide ange o applica ions. 477 - The esul s ob ained in his wo k show ha he ma e ial eco e ing o he polyme ic esin in 478 he CFRP was e ecycling p ocess is possible, which ep esen s a conside able ad ance in he 479 ield. This is go by a echnically simple and scalable me hod, e y usual in he chemical indus y. 480 As a as cos s a e conce ned, he only ele an cos is he ene gy consump ion o each he 481 ea men empe a u e, since solid bed ma e ial is a eusable was e ma e ial. Besides, his 482 ene gy could be ob ained om he gases h ough he sepa a ion o H2 by p essu e swing 483 adso p ion (PSA) and he employmen o he by-p oduc gas, which would e ain high HHV, o 484 gene a e ha ene gy. 485 486 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64 65 19 Acknowledgemen s 487 The au ho s wan o hank he Minis y o Economy and Compe i i eness o he Spanish 488 Go e nmen o he unding (Re . CTM2013-48887-C2-1-R). The au ho s also hank he Basque 489 Go e nmen o he Resea che T aining G an awa ded o N. 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