LV11751B - Method for production of cellulose - Google Patents

Abstract

The invention concerns the cellulose for chemical processing, methods of producing microcrystalline and powder-like cellulose from the lignocellulose. This method of production of nitrocellulose and products based on it is useful for the following industries: cellulose/paper industry, chemical, food, and perfume industries.The aim of this invention is to shorten the time of the delignification process and to increase the quality of the final product, which is produced by explosive delignification of the pulverized raw material, heating it in a reactor with water vapour for a certain time under the final temperature, ejecting the material and segregating the cellulose with the help of an alkaline agent.The novelty of the invention is that before placing the raw material into a reactor, it gets saturated with nitric acid, and the heating is conducted under a temperature of 165-200 degrees C for 30-55 seconds. It is advisable to saturate the raw material with a compound consisting of nitric acid and 20-60% ethyl alcohol, or adding to those two components one of the following acids: H2SO4, HCl, H3PO4, while conducting heating with water vapour mixed with 20-60% ethyl alcohol vapour.

Description

II: II: LV 11751

Cnocoā ποπγΜθΗΜΗ LļennK) no3bi M3o6peTeHne οτηοομτοα k cnocočaM ποπυηθημη i_ļenmono3bi nna xnivinHecKoii nepepačoTKu, nonyHeHUfl MHKpoKpucTannuHecKOH v \ ποροιυκοΒΟΜ Liennrano3bi M3 nnrHOLienmono3Horo cbipbfl, npenMymecTBeHHO H3 πμοτβθηηομ ApeeecMHbi. Cnoco6 Lļenecoo6pa3HO ncnonb30BaTb b Lļenniono3Ho-6yMa > t < HOM npon3BOflCTBe, XHMHHeCK0M, nHlHeB0ii, ΠθρφίΟΜθρΗΟίί npOMbllUneHHOCTM, B ΤΘΧΗΟΠΟΓΙΊΜ ΠΟΠγΗΘΗΗΗ HHTpoL (enniono3bi. B τόμ μμοπθ npn npon3BOACTBe HmpaTOB uenjiiono3bi n προηγκτοΒ Ha I ocHOBe. M3BecTeH cnoco6 ποπυηθημη ποροιυκοΒοιζι ι / ι MkiKpoKpi / iCTannunecKOM uenmono3bi πγΤΘΜ B3pblBHOrO aBTOrHflpOnH3a, ΠΟ KOTOpOMy H3MenbHeHHbm jinmouenniono30coiļep) Kamma? i MaTepnan 3arpyxaioT b PEAKTOP BbicoKoro AAB / ieHMH, HarpeBaioT ao 185-240 ° C m 'BbicTpemīBaiOT "πγτθΜ pe3Koro οημχθημη α3Βπθημα; ποπγπβΗΗγκ) Maccy pa3AenflioT Ha uenniono3y, reMMuenmono3bi μ πμγημη, 3aieM OTAermioT uenmono3y, nponmbiBaioT ee oahom M3 khchot rpynnbi HCI, H2S04 (S02) n ΒτορΜΗΗΟ noABepraioT B3pbiBH0My aBTornAponn3y.nonyHeHHyio Maccy oxna > kaai, HeMTpaAM3yK) T μ οτΑβπΗίοτ κοηθμηνη προΑγκτ. (11a. KaHaAbi # 1198703, C08 B 1/00, C13k1 / 02.1985). Ηθαοοτθτοκ cnocoča-MHorocTaAniiHOCTb npopecca μ ημ3κοθ KanecTBO nonynaeMoro προΑγκτβ.

Han6onee 6πμ3ΚΜΜ of τθχημμθοκομ cymHocTM m AOCTMraeMOMy pe3ynbTaTy ίΐΒΠΑβτοη cnocoč ποπγπθΗΜΗ ΜίικροκρΜοτθΑπί / h ΐΗθΟκοίί ποροιυκοΒοίί Menniono3bi ΠγΤΘΜ B3pblBHOrO 3ΒΤ0ΓΜΑΡ0ΠΜ33 Μ3Μ6ΠΒ4ΘΗΗ0Γ0 ΑΘΠΠΙ0η03000Αβρ > ΙΟ111ΘΓ0 Cbipbfl ΠρΜ HarpeBe ero b PEAKTOP BOA ^ HbiM napoM ao 205-250 ° C 3a 30-35c, βηαθρχκομ ao 15 ΜΜΗγτ npn 3τοίί TeMnepaType "BbicTpenoM" c ποοπθαυιοιαμμ BbiAeneHHeM peneBoro npoAyKTa, B03AeiicTBneM Ha Maccy ιαθπομηνμ areHTOM, npoMbiBKoū boaoīi m 0T6ennBaHneM.OAHaK0 ποπυηθηηθη τθκμμ οποοο6ομ uenmono3a ημθθτ HH3Kyio 2 cTeneHb nonnMepu3aqnn n 6onbwyio jviMTenbHocTb npouecca B3pbiBHoro aBTornflponn3a (ABTopcKoe CBMfleTe / ibCTBO # 1,792,942, Oct. 8. 1992r)

M3oCpeTeHHii-coKpau4eHMe flnuTenbHocTM npouecca aenvHV < pmaL m n noBbiiueHMe KanecTBa κοηθμηογο npoflyicra. riocTaBneHHafl uenb flocTuraeTca M38ecTHbiM cnocočoM nonyHeHMfl uennio / io3bi B3pbiBHbiM aBTornflponM30M n3MenbMeHHoro uennK3no30COflepxamero cbipbSR npn HarpeBe ero b PEAKTOP BOfliiHbiM napoM, Bbiflep > CEE npn κοΗΘΗΗοίί TeMnepaType "BbicTpenoM" Maccbi n BbifleneHneM H3 Hee uenntono3bi menoHHbiM areHTOM, b κοτοροΜ b otnmm οτ M3BecTHoro cnocoča, cbipbe nepefl HarpeeoM b peaicrope npeflBapmenbHO nponmbiBatoT a30THoti κκοποτοίί, napoBoii Harpee ββριγτβο 165-200 ° C n Bbiflep > KK npn 3τοίί TeivinepaType 30-55c; npeONHTMTenbHee nponnTKy cbipbH secTH CMecbto a30TH0ii KucnoTbi c 20-60% θτμ / ιοβογο cnupTa, m ia 3aHHiii CMecbra c AočaBneHneM oahoPi KucnoTbi m rpype H 2 SO 4 HCl, H 3 PO 4. TaioKe npeflnoMTmenbHee HarpeBaHue cbipbfl b headKTope βθοτμ CMecbto napoe BOflb c 20-60% napoB 3TnnoBoro cnup. Αοοτμχθημθ τθχηιίηθοκογο pe3ynbTaī CBfl3aHo c 33ΑΒΠθηηομ coBOKynHocTbto cymecTBeHHbix npn3HaKOB cneflyrotanM očpa30M.

ripeflBapMTenbHafl nponuTKa cbipba a30THoti ΚΜοποτοίί ρβ3κο MHTeHCMcf) MUkipyeT 0KMcnnTenbHyra flecTpyKuwo numnHa, HacTMHHoe ero HHTpoBaHMe n rnflponnTMHecKyio flecTpyKumo reMMuenmono3, a TeMnepaTypa HarpeBa cbipba b PEAKTOP b npenenax 165-200 ° C npuBOflm κ yBenn4eHnro nnacTMMHocTM nnrHoyrneBOAHoīi MaTpuubi. ripnseM uenniono3Ha5i cocTaBrmiomafl cbipbfl npn stom reMnepaType coxpaH "eT cboio > xecTKOCTb, B pe3ynbīaie nePicTBua 3thx cļjaKTopoB- nponuTKu a30THoPi kuchotom w cnvoKenm TeMnepaTypbi HarpeBa b PEAKTOP, npw noc / ieflyK > MEM" BbiCTpene "pa3BonoKHeHne pacTmenbHoro cbipba nponcxonnT NPH MeHbmePi ΒρβΜβΗΗοίί Bbiflepx < Ke h uenriiono3a OKa3biBaeTCB μθηθθ noBpe > KAeHHoii.nocneflyroiiiafl HHKy6aumb pa3BonoKHeHHoii Maccbi cnocočcTByeT flanbHeiiluePi flecTpyKUnn nnmoyrneBOflHoro KOMnneKca c o6pa30BaHneM nponyKTOB, pacTBopwvibix b BOflHbix pacTBopax menoHK, a npoTeKaiomHPi napannenbHO n / inponmmecKm npouecc BbicoKOMoneKynapHoii Mac ™ uejinrano3bi cnoco6cTByeT nonyHeHHto 6-one oflHopoflHoro ueneeoro npoflyKTa, npnroflHoro KaKfl / ia xnMUHecKofi do not read, TaK 3 3 EN 11751 m flna nonyHeHM «ποροΐϋκοΒΟΜ μ MMKpoKpucTannuHecKOM uenJiiono3bi. CoKpameHne Bbiflep > KKM cbipba b peaicrope, HBnntomeMcn nMMMTMpyiomeM CTaflueii npoLiecca, no. Jļo6aBneHne napoB θτμποβογο cnupTa κ BOflflHbiM napaM cnoco6cTByeT αοοτηχθημιο 6-one βηοοκμχ αθβπθημμ b μμκροοκοπμηθοκμχ o6nacTnx flpesecHoii κηβτκΜ npn MeHbiunx TeMnepaiypax, whereby to TaiOKe cnocoācTByeT coKpaineHMio ΒρβΜβΗΜ flenurHi / icfiMKauMU cbipbfi b PEAKTOP. wheel nponuTKe cbipba a30THoti κμοποτομ c fločaBKoii cnupTa, a TaiOKe 3anBneHHbix noāaBOK MMHepanbHbix KucnoT Π03Β0ΠΛΚ3Τ perymipoBaTb conepaoHMe Heuenniono3Hbix ΚΟΜΠΟΗΘΗΤΟΒ B ΚΟΗΘΗΗΟΜ ΠρΟβγΚΤΘ B 3aBMCMMOCTM OT ΘΓΟ ΠρΑΜΟΓΟ Ha3HaHeHMfl M HCXOflHOrO Cbipbfl. 3ayiBJieHHbm cnocoč ocymecTBnneTcn cneflyioiunM o6pa30M.

TexHo / iornHecKyio menu npe / enBenTenbHO npouTbieaioT BapoHHbiM PacTBopoM B κθηθοτβθ BapoHHoro pacTBopa ncnonb30Ba / in 6-12% BOflHbie pacTBopb a30TH0M KMCnOTbl. PaCTBOpbl a30TH0M KMCHOTbl CflOBKaMM CepHOM KMCnOTbl (1-2%) M STunoBoro cnupTa (40%) aB / iaioTca ohmm H3 BapnamoB BapoHHoro pacTBopa. ΠροπΜτκγ menbi npoBOflunu neyMa cnocočaMM. Πο nepBOMy cnoco6y meny Bbipep &kt; KHBaiOT b τθηθημθ 8 nacoB npn Monyne 1: 3-1: 5, nocne nero M3aBiTOK pacTBopa ynanntOT. ΒτοροΡί cnoco6 προπμτκμ 3aKnioHaeTCfl b tom, hto προβοαητ nnTb μμκποβ npeccoBaHMfl menbi bapoHHOM pacTBope. Umkji npeccoBanna βκπιοηθθτ Bbiflep KKy menbi nofl αθβπθημθμ 8Mna b τθηθημθ 1 mmh, m BbinepxKy npn aTMoccfeepHOM ΑΘΒπθημμ b τθηθημθ 1 mmh m Mony 1: 3-1: 5, nocne nero M36biTOK KMcnoTbi οιμβθιοτ. ApροπΜΤθΗΗγιο BapoHHbiM pacTBopoM meny 3arpy > xai0T b npeflBapMTenbHo HarpeTbiM UMnMHfpMHecKMM HeadKop. PeaKTop γθρμθτμηηο 3aKpbieaioT m HanonHnioT HacbimeHHbiM napoM 3anaHH0M TeMnepaTypbi. noflteM TeMnepaTypbi b peaKTope ocymecTBnneTcn b τθηθημθ 10-30c. BpeMn BbiflepacKM b peaKTope OTCHMTbiBaiOT c μομθητθ flocTMxeHMfl 3aflaHH0M TeMnepaTypbi. ΠοοτοηΗΗΟΘ flaeneHMe napa b peaicrope noflflep > KMBaioT flononHMTenbHbiM bboaom He6onbiiJMX κοπμηθοτβ napa.no μοτθηθημμ ΗβοδχοΑΜΜοτο βρθμθημ c noMoiiļbio napOBoro KpaHa προΒΟβητ μγηοβθηηνμ c6poc flaBneHMfl- neKOMnpeccMKD, b pe3ynbTaTe nero flpeeecHan Macca "BbicTpenMBaeTcn" b cčopHMK. CοπγπΘΗΗγιο Maccy npoMbieatoT boaom, a 3θτθμ noflBepraioT SKCTpaKUMM 0.1-5% -HbiM pacTBopoM ιαθποηηογο areHTa npM TeMnepaType 4

II from 100 ° C πpoflon > KHTenbHOCTbio no onHoro Match c noBTopflrameiicfl ποΒΤορΗοίί npOMbIBKOM.

Cnoco6 nnmocTpnpyeTCfl cnenyiomnMM npuMapiv. B KanecTBe npmviepoB npuBonsiTCii nanHbie aKcnepmvieHTOB, KOTopbie npuBeneHbi no luckHHiii ïχθμθ, ho npn pa3nnHHbix 3HaHeHHHx napaMeTpoB cnocoča. McxonHbie naHHbie m pe3ynbTaTbi 3tmx aKcnepmvieHTOB OTpax < eHbi b Tačnme. B KanecTBe qenniono3oconepxainero cbipbi? b npmviepax # 1-4 TačnuLilbi ncnonb30Bann 6epe30Byio meny, b npmviepe # 5-cocHOByra meny. 5LV 11751 IH / IHECKME flAPAMETPbl ΠΡΟΜΕΟΟΑ B3PblBHOI / l ΑΕΠΜΓΗΜΦΜΚΑΜΜΜM XAPAKTEPMCTMKA UEnflK) n03bl

X o cc z 2 o Q_ O C h h 0 C o o o. Yo 1 0? CM cc s X- * c Q * * CD co 540 780 830 1 980 1 X SX (C * o. Ω a: o O 1 o 5 2 c (βω «= is LO C 00 o co co co σ '- x ~ s X L_ s LO o CM CO o o o o co o σ > co o O-P | 11-ω S' zr C CO CO. 0) - CB c ω r2 ms £ a 1 2 cc co 00 c CM Λ S CL _ or > 5 ¥ i-2 to ir. Ο υ υ α g ο m = c -0 5 1 Lo LO LO LO LO LO O CO CC [ψ * S 5 ° ° - I 2 g O 1 hc H o CO o LO o LO lsi 1 č " o N oo (M LO LO CO LO C- ca cu cc O g- cS c 3 Ο O-r? O o ca o o o o X X X X X X X X X X fl fl fl fl fl i X X X § ω _ cc X * < o f'l CQ O 4 o 2: x 8 xj 8 3 g g-bg ^ g X m O o 4o 2 X (Λ T = < m ™ ggg co O z X (M co oz X vp CM CO oz X CM% - CM CO LO 6 LV 11751

Oopi \ / iyna μ3ο6ρθτθημα 1 Cnocoč ΠΟΠγΗΘΗΜΑ LļeJint0n03bl ΠγΤβΜ B3pblBHOM ΗΘΠΜΓΗΙΐφΐ / ΙΚ314ΜΜ M3MenbHeHHOrO ΠΜΓΗΟί4ΘΠΠΚ) Π03ΗΟΓΟ Cbipbfl, BKJKOHaiOmtlii Η3ΓρβΒ3ΗΜΘ ΘΓΟ B PEAKTOP βοαηηημ napoM, Bbiflep > KKy npn κοηθηηομ TeMnepaiype "BbicTpen" Maccbi M3 PEAKTOP, BbifleneHMe ee W3 Lļenniono3bi menoHHbiM areHTOM m npoMbiBKy ee Bofloii, omuHarainuMca τθμ, hto c uejibto coKpameHna flnmenbHocTH npopecca flennrHn0HKaunn n noBbiLueHna KanecTBa κοηθηηογο npoflyKTa, cbipbe nepefl HarpeBOM b PEAKTOP npeflBapuTenbHO nponuTbiBatoT a30THoii κΜοποτοιί, a napoBoPi HarpeB Ββργτ flo 175-200 ° c n Bbiflep > KHBaK) T npn stom TeMnepaType 30 -55c. 2. Cnocoč no n.1, OTnunarainnkicii τθμ, hto cbipbe nponuTbiBatoT cMecbto a30THoii KUcnoTbi c 20-60% 3τμποβογο cnupTa. 3. Cnocoč from n ou 2, oTHMHaioiflMiicfl τθμ, hto Cbipbe nponuTbiBatoT cMecbto a30THoPi KucnoTbi c 20-60% STunoBoro cnupia c AočaBneHneM oflHoii H3 KucnoT rpynnbi H2SO4, HCl, H3PO4. 4. Cnocoč of n.1. OTnuHaiomniicH τθμ, hto HarpeB nponmaHHoro cbipbfi b peaKTope Ββηγτ cMecbto napoB BOflb c 20-60% napoB θτμποβογο cnHpTa.

PecpepaT H30ČpeTeHMe othochtch cnocočaM nonyneHHH uenntono3bi flJifl χμμμηθοκομ nepepčoTKM ΜΜκροκρνιοτΒππιΐΗβοκοΫι n nopomKOBoPi uennK) no3bi H3 nnrHoqennK) no3Horo cbipbfl. Cnocoč Lienecoočpa3HO ncnonb30BaTb b uenniono3Ho-cyMaxHOM npon3BOflCTBe, xnMHHecKOki, nmneBoPi n πβρφιοΜβρΗΟΗ npoMbiiiHHOCTH, b τθχηοπογμμ nonyneHHB HHTpouenmono3bi n προηγκτοΒ Ha ee ocHOBe. Lenbeb H30cpeTeHHH-coKpHenHHNTM npouecca flennrHi ^ HKaqnn h noBbiiiHne KanecTBa κοηθηηογο nponyKTa. 3aHBneHHbiii TexHnnecKnii pe3ynbTaT flocwaeTca cnocočoM B3pbiBHoiži flenMn-u ^ HKaflHH n3MenbHeHHoro nnmouenniono3Horo cbipbfl npn HarpeBe ero b PEAKTOP BOflflHbiM napoM, Bbiflep > CEE NPH κοηθηηομ TeMnepaType "BbicTpenoM" Maccbi v \ BbineneHHH H3 Hee uenmono3bi menoHHbiM areHTOM. Cbipbe nepen HarpeBaHMeM b peaKTope npeflBapurrenbHO nponMTbiBaeTcsi a30TH0ki KucnoToii, napoBoii HarpeB Ββπγτ flo 165-200 ° C h Bbiflep > KK πρι / ι 3τοίί TeMnepaType 30-55c; npeflnoHTHTenbHee προπΜτκγ cbipbfl ocyiflecTBnsiTb CMecbto c fločaBneHMeM oflHoti KHcnoTbi m rpynnbi H 2 SO 4) HCl, H 3 PO 4, a napoBoii HarpeB npoBOflMTb TaioKe CMecbto napoB BOflb c 20-60% napoB 3τμποβογο cnupTa.

Claims (4)

A method for producing a pulp by explosively delignifying the crushing of lignocellulose raw materials, which includes heating the reactor with water vapor, to end temperature, mass " shooting " characterized in that, in order to shorten the duration of the delignification process and to increase the quality of the final product, the feedstock is pre-heated with nitric acid prior to heating in the reactor, steam heating is carried out to 175-200 ° C. C and stand at this temperature for 30-55 s. Method according to claim 1, characterized in that the raw material is impregnated with a mixture of nitric acid and 20-60% ethyl alcohol. Method according to claim 1 or 2, characterized in that the raw material is impregnated with a mixture of nitric acid and 20-60% ethyl alcohol by adding one acid from the group H2SO4, HCl, H3PO4. Method according to claim 1, characterized in that the heating of the impregnated feedstock in the reactor is carried out with a steam mixture containing water vapor and 20-60% ethyl alcohol vapor.