Abstract:Kuitira kutsiva iyo isingaparadzike polyvinyl doro (PVA) slurry, hemp stalk cellulose ether-hydroxypropyl methylcellulose yakagadzirwa kubva kune ekurima tsvina hemp mashanga, uye yakasanganiswa nechaiyo starch kugadzirira slurry. Polyester-donje yakasanganiswa shinda T/C65/35 14.7 tex yakanga yakakura uye kuita kwayo saizi kwakaedzwa. Iyo yakakwana yekugadzira nzira ye hydroxypropyl methylcellulose yaive inotevera: chikamu chikuru che lye chaive 35%; iyo compression ratio yealkali cellulose yaive 2.4; The liquid volume ratio ye methane uye propylene oxide ndeye 7: 3; dilute ne isopropanol; iyo reaction pressure ndeye 2. 0MPa. Saizi yakagadzirwa nekusanganisa hydroxypropyl methylcellulose uye chaiyo starch ine yakaderera COD uye ine hushamwari hwakatipoteredza, uye ese masaizi zviratidzo anogona kutsiva PVA saizi.
Mazwi akakosha:hemp stalk; hemp stalk cellulose ether; polyvinyl doro; cellulose ether sizeng
0.Nhanganyaya
China ndiyo imwe yenyika dzine zviwanikwa zvemashanga zvakapfuma. Goho rinodarika matani 700 miriyoni, uye kushandiswa kwemashanga kunongova 3% pagore. Huwandu hwezviwanikwa zvehuswa hahuna kushandiswa. Mashanga akapfuma echisikigo lignocellulosic mbishi zvinhu, izvo zvinogona kushandiswa mukudya, fetiraiza, cellulose derivatives uye zvimwe zvigadzirwa.
Parizvino, kushuvira kusvibiswa kwemvura yetsvina mukugadzira machira kwave imwe yenzvimbo huru dzekusvibisa. Iyo kemikari oksijeni inoda yePVA yakanyanya. Mushure mekunge mvura yetsvina yeindasitiri inogadzirwa nePVA mukudhinda uye kudhayira yaiswa murwizi, inodzivisa kana kutoparadza kufema kwezvipenyu zvemumvura. Uyezve, PVA inowedzera kuburitswa uye kutama kwesimbi inorema mumiviri yemvura, zvichikonzera matambudziko akanyanya ezvakatipoteredza. Kuita tsvakiridzo yekutsiva PVA negirinhi slurry, zvinodikanwa kwete chete kuzadzisa izvo zvinodikanwa zvekuita saizi, asi zvakare kudzikisa kusvibiswa kwemvura nemhepo panguva yekuita saizi.
Muchidzidzo ichi, hemp stalk cellulose ether-hydroxypropyl methylcellulose (HPMC) yakagadzirirwa kubva kumarara ekurima hemp mashanga, uye maitiro ayo ekugadzira akakurukurwa. Uye sanganisa hydroxypropyl methylcellulose uye saizi chaiyo yesitashi sehukuru hwekuyera, enzanisa nePVA saizi, uye kurukura kuita kwayo saizi.
1. Kuedza
1 . 1 Zvishandiso uye zviridzwa
Hemp stalk, Heilongjiang; polyester-cotton yakasanganiswa shinda T/C65/3514.7 tex; akazvigadzira hemp stalk cellulose ether-hydroxypropyl methylcellulose; FS-101, yakagadziridzwa starch, PVA-1799, PVA-0588, Liaoning Zhongze Group Chaoyang Textile Co., Ltd.; propanol, premium giredhi; propylene oxide, glacial acetic acid, sodium hydroxide, isopropanol, analytically yakachena; methyl chloride, yakakwirira-kuchena nitrogen.
GSH-3L reaction kettle, JRA-6 dhijitari inoratidzira magineti inobvongodza mvura yekugezera, DHG-9079A yemagetsi inodziya inogara tembiricha yekuomesa oveni, IKARW-20 pamusoro pemechani agitator, ESS-1000 sampuli saizi muchina, YG 061/PC yemagetsi imwe yarn simba mita , LFY-109B yekombuta abrasion tester.
1.2 Kugadzirira kwehydroxypropyl methylcellulose
1. 2. 1 Kugadzirira kwe alkali fiber
Kamura dzinde rehemp, pwanya kusvika pamakumi maviri meshes ne pulverizer, woisa hupfu hwehemp kune 35% NaOH aqueous solution, woinyika pakamuri tembiricha kwe1. 5 ~ 2 . 0 h. Svina iyo yakaiswa alkali fiber kuitira kuti huwandu hwehuwandu hwealkali, cellulose, nemvura huve 1. 2: 1. 2:1.
1. 2. 2 Etherification reaction
Kanda alkali cellulose yakagadzirwa mukettle inopindura, wedzera 100 mL ye isopropanol se diluent, wedzera mvura 140 mL yemethyl chloride uye 60 mL yepropylene oxide, vacuumize, uye simbisa kusvika ku2. 0 MPa, zvishoma nezvishoma simudza tembiricha kusvika 45 ° C kwemaawa 1-2, uye ita pa 75 ° C kwemaawa 1-2 kugadzirira hydroxypropyl methylcellulose.
1. 2. 3 Post-processing
Gadzirisa pH ye etherified cellulose ether ine glacial acetic acid kusvika ku6. 5 ~ 7 . 5, yakashambidzwa nepropanol katatu, uye yakaomeswa muovheni pa85°C.
1.3 Kugadzira maitiro ehydroxypropyl methylcellulose
1. 3. 1 Mhedzisiro yekutenderera kumhanya pakugadzirira kwe cellulose ether
Kazhinji etherification reaction ndeye heterogeneous reaction kubva mukati kuenda mukati. Kana pasina simba rekunze, zvakaoma kuti etherification agent ipinde mukristallization ye cellulose, saka zvakakosha kubatanidza zvakakwana etherification agent ne cellulose nenzira yekukurudzira. Muchidzidzo ichi, high-pressure yakasimudzwa reactor yakashandiswa. Mushure mekuedza kwakadzokororwa uye kuratidzwa, iyo yakasarudzwa yekutenderera kumhanya yaive 240-350 r/min.
1. 3. 2 Mhedzisiro yealkali concentration pakugadzirwa kwe cellulose ether
Alkali inogona kuparadza iyo compact chimiro che cellulose kuti iite kuzvimba, uye kana kuzvimba kweamorphous dunhu uye crystalline dunhu rinowanzoenderana, iyo etherification inofamba zvakanaka. Mukugadzirwa kwe cellulose ether, huwandu hwealkali hunoshandiswa mu cellulose alkalization process ine simba guru pakubudirira kwe etherification yezvigadzirwa zveetherification uye dhigirii rekutsiva mapoka. Muchigadziro chekugadzirira kwehydroxypropyl methylcellulose, sezvo kuwedzera kwe lye kunowedzera, zvinyorwa zvemethoxyl mapoka zvinowedzerawo; Ukuwo, kana iyo yakadzikira yelye inoderera, iyo hydroxypropyl methylcellulose Iyo yekutanga yemukati yakakura. Zviri muboka remethoxy zvakananga kuenzana nekugadzirisa lye; zviri mukati me hydroxypropyl zvakapesana nekuwanda kweiyo lye. Chikamu chikuru cheNaOH chakasarudzwa se35% mushure mekuedzwa kwakadzokororwa.
1. 3. 3 Mhedzisiro yealkali cellulose kudzvanya reshiyo pakugadzirwa kwe cellulose ether.
Chinangwa chekutsikirira alkali fiber ndechekudzora mvura yealkali cellulose. Kana chiyero chekutsikirira chiri chidiki zvakanyanya, huwandu hwemvura hunowedzera, kuwanda kwe lye kunoderera, chiyero cheetherification chinodzikira, uye etherification agent inogadzirwa nehydrolyzed uye maitiro epadivi anowedzera. , iyo etherification inoshanda yakaderera zvakanyanya. Kana iyo reshiyo yekudzvanya yakakurisa, iyo yemvura inodzikira, iyo cellulose haigone kuzvimba, uye isina reactivity, uye iyo etherification agent haigone kusangana zvizere nealkali cellulose, uye mhinduro haina kuenzana. Mushure mekuedzwa kwakawanda uye kudzvanya kuenzanisa, zvakatemwa kuti huwandu hwehuwandu hwealkali, mvura uye cellulose yaive 1. 2: 1. 2:1.
1. 3. 4 Mhedzisiro yekushisa pakugadzirwa kwe cellulose ether
Mukugadzira hydroxypropyl methylcellulose, tanga wadzora tembiricha pa50-60 ° C uye uichengete patembiricha isingaperi kwemaawa maviri. Iyo hydroxypropylation reaction inogona kuitwa panenge pa30 ℃, uye iyo hydroxypropylation reaction rate inowedzera zvakanyanya pa50 ℃; zvishoma nezvishoma simudza tembiricha kusvika 75 ℃, uye dzora tembiricha kwemaawa maviri. Pa 50 ° C, iyo methylation reaction haigone kuita, pa60 ° C, chiyero chekuita chinononoka, uye pa75 ° C, iyo methylation reaction rate inokurumidza zvikuru.
Kugadzirira kwehydroxypropyl methylcellulose ine-multi-stage tembiricha yekudzora haingodzore kuenzana kwemethoxyl uye hydroxypropyl mapoka, asi zvakare kubatsira kuderedza maitiro epadivi uye mushure mekurapa, uye kuwana zvigadzirwa zvine hungwaru chimiro.
1. 3. 5 Mhedzisiro ye etherification agent dosage ratio pakugadzirwa kwe cellulose ether
Sezvo hydroxypropyl methylcellulose iri yakajairika isiri-ionic yakasanganiswa ether, mapoka emethyl nehydroxypropyl anotsiviwa pane akasiyana hydroxypropyl methylcellulose macromolecular cheni, kureva, C akasiyana mune yega yega glucose mhete. Kune rimwe divi, chiyero chekugovera chemethyl uye hydroxypropyl ine kupararira kukuru uye kusarongeka. Kunyungudika kwemvura kweHPMC kune hukama nezviri mukati methoxy boka. Kana zvinyorwa zvemethoxy boka zvakaderera, zvinogona kunyungudutswa mune yakasimba alkali. Sezvo methoxyl yemukati ichiwedzera, inova yakanyanya kunzwisiswa nekuzvimba kwemvura. Iyo yakakwirira iyo methoxy yemukati, zviri nani kunyungudika kwemvura, uye inogona kugadzirwa kuita slurry.
Huwandu hweetherifying agent methyl chloride uye propylene oxide ine mhedzisiro yakananga pane zviri mukati methoxyl uye hydroxypropyl. Kuti ugadzirire hydroxypropyl methylcellulose pamwe nekunyungudika kwemvura kwakanaka, iyo liquid volume reshiyo yemethyl chloride uye propylene oxide yakasarudzwa se7:3.
1.3.6 Iyo yakakwana yekugadzira maitiro ehydroxypropyl methylcellulose
The reaction equipment is a high-pressure stirred reactor; kukurumidza kutenderera ndeye 240-350 r / min; chikamu chikuru chelye ndicho 35%; the compression reshiyo yealkali cellulose i2. 4; Hydroxypropoxylation pa50 ° C kwemaawa maviri, methoxylation pa75 ° C kwemaawa maviri; etherification agent methyl chloride uye propylene oxide liquid volume reshiyo 7: 3; vacuum; pressure 2 . 0 MPa; diluent is isopropanol.
2. Kuonekwa uye kushandiswa
2.1 SEM yehemp cellulose uye alkali cellulose
Tichienzanisa iyo isina kurapwa hemp cellulose uye iyo hemp cellulose yakarapwa ne35% NaOH, zvinokwanisa kuwanikwa pachena kuti alkaliized cellulose ine matsemuka akawanda epamusoro, nzvimbo yakakura yepamusoro, chiitiko chepamusoro uye nyore etherification reaction.
2.2 Infrared Spectroscopy Kutsunga
Iyo cellulose yakabviswa kubva kumande ehemp mushure mekurapwa uye infrared spectrum yeHPMC yakagadzirwa kubva kuhemp stalk cellulose. Pakati pavo, iyo yakasimba uye yakafara bhendi yekunyura pa 3295 cm -1 ndiyo inotambanudza vibration absorption bhendi yeHPMC kusangana nehydroxyl boka, bhendi rekunyudza pa1250 ~ 1460 cm -1 ndiro bhendi rekunyudza CH, CH2 uye CH3, uye kunyura. bhendi pa1600 cm -1 ndiro bhendi rekunyudza remvura mubhendi repolymer absorption. Bhandi rekunyudza riri pa1025cm -1 ndiro bhendi rekunyudza reC - O - C mupolymer.
2.3 Viscosity kutsunga
Tora iyo yakagadzirwa cannabis stalk cellulose ether sample woiwedzera mubeaker kugadzirira 2% aqueous solution, kurunga zvakanaka, kuyera viscosity yayo uye viscosity kugadzikana ne viscometer, uye kuyera avhareji viscosity ka3. Iyo viscosity yeyakagadzirirwa cannabis stalk cellulose ether sampu yaive 11. 8 mPa·s.
2.4 saizi application
2.4.1 Slurry kugadzirisa
Iyo slurry yakagadzirirwa mu 1000mL ye slurry ine chikamu chikuru che 3.5%, yakavhenganiswa pamwe chete nemusanganisi, ndokuzoiswa mumvura yekushambidza nemvura uye inopisa kusvika 95 ° C kwe 1 h. Panguva imwecheteyo, cherechedza kuti pulp yekubika ndiro inofanira kuvharwa zvakanaka kudzivirira kusanganiswa kweslurry kubva pakuwedzera nekuda kwekubuda kwemvura.
2.4.2 Slurry kuumbwa pH, miscibility uye COD
Sanganisa hydroxypropyl methyl cellulose uye saizi chaiyo yestarch kugadzirira slurry (1#~4#), uye enzanisa nePVA formula slurry (0#) kuti uongorore pH, miscibility uye COD. Iyo polyester-donje yakasanganiswa shinda T/C65/3514.7 tex yaive saizi pamushini weESS1000 saizi yemuchina, uye kuita kwayo saizi yakaongororwa.
Zvinogona kuonekwa kuti hemp stalk stalk cellulose ether uye saizi chaiyo yestarch 3 # ndiyo yakanyatsogadzirwa saizi: 25% hemp stalk cellulose ether, 65% yakagadziridzwa starch uye 10% FS-101.
Yese saizi data inofananidzwa nesaizi data yehukuru hwePVA, zvichiratidza kuti saizi yakasanganiswa yehydroxypropyl methylcellulose uye chaiyo starch ine kuita kwakanaka saizi; pH yayo iri pedyo nekusarerekera; hydroxypropyl methylcellulose uye starch chaiyo COD (17459.2 mg / L) yehukuru hwakavhenganiswa hwe starch hwakanyanya kuderera kupfuura iyo yePVA size (26448.0 mg / L), uye kushanda kwekuchengetedzwa kwezvakatipoteredza kwaive kwakanaka.
3. Mhedziso
Iyo yakakwana yekugadzira maitiro ekugadzira hemp stalk cellulose ether-hydroxypropyl methylcellulose yekuisa saizi ndeiyi inotevera: yakanyanya-kudzvanywa yakasimudzwa reactor ine kutenderera kumhanya kwe240-350 r/min, chidimbu chidimbu chelye ye35%, uye compression reshiyo. yealkali cellulose 2.4, tembiricha yemethylation i75 ℃, uye tembiricha yehydroxypropylation i50 ℃, imwe neimwe inochengetwa kwemaawa maviri, iyo liquid volume reshiyo yemethyl chloride uye propylene oxide iri 7:3, vacuum, iyo reaction pressure i2.0 MPa, isopropanol ndiyo diluent.
Hemp stalk cellulose ether yakashandiswa kutsiva PVA size ye size, uye optimal size reshiyo yaive: 25% hemp stalk cellulose ether, 65% yakagadziridzwa starch uye 10% FS-101. Iyo pH ye slurry ndeye 6.5 uye COD (17459.2 mg / L) yakanyanya kuderera kupfuura iyo yePVA slurry (26448.0 mg / L), inoratidza kushanda zvakanaka kwezvakatipoteredza.
Hemp stalk cellulose ether yakashandiswa kuyera pachinzvimbo chePVA saizi kuyera polyester-donje yakasanganiswa shinda T/C 65/3514.7tex. Iyo saizi index yakaenzana. Iyo itsva hemp stalk cellulose ether uye yakagadziridzwa starch yakasanganiswa saizi inogona kutsiva PVA saizi.
Nguva yekutumira: Feb-20-2023