CMC Cellulose uye Chimiro Chayo Chimiro

Ichishandisa mashanga cellulose seyakagadzirwa, yakagadziridzwa ne etherification. Kuburikidza nechinhu chimwe chete uye bvunzo yekutenderera, iyo yakakwana mamiriro ekugadzirira kwecarboxymethyl cellulose yakatemerwa kuve: etherification nguva 100min, etherification tembiricha 70.℃, NaOH dosage 3.2g uye monochloroacetic acid dosage 3.0g, iyo yakanyanya kutsiva Iyo degree ndeye 0.53.

Mazwi akakosha: CMCcellulose; monochloroacetic acid; etherification; modification

Carboxymethyl cellulosendiyo inonyanya kugadzirwa uye inotengeswa serulosi ether pasi rose. Inoshandiswa zvakanyanya mukuchenesa, chikafu, mushonga wemazino, machira, kudhinda uye dhayi, kugadzira mapepa, peturu, migodhi, mishonga, ceramics, zvigadzirwa zvemagetsi, rabha, Paints, mishonga yezvipembenene, zvizoro, dehwe, mapurasitiki nekuchera mafuta, nezvimwe, zvinozivikanwa. se "industrial monosodium glutamate". Carboxymethyl cellulose imvura inonyungudika selulosi ether inotorwa nekugadzirisa makemikari cellulose. Cellulose, iyo huru mbishi yekugadzirwa kwecarboxymethyl cellulose, ndeimwe yezvakawanda zvechisikigo zvinogonekazve pasi pano, nekugadzirwa kwepagore kwemazana emabhiriyoni ematani. nyika yangu inyika huru yekurima uye imwe yenyika dzine huswa hwakawanda. Mashanga agara ari mamwe emafuta makuru ekurarama kune vagari vekumaruwa. Zviwanikwa izvi hazvina kugadzirwa kwenguva yakareba, uye isingasviki 2% yemarara ekurima nemasango semashanga anoshandiswa munyika gore rega rega. Mupunga ndicho chirimwa chikuru chehupfumi mudunhu reHeilongjiang, ine nzvimbo yekudyara inodarika mamirioni maviri hm2, gore negore goho rematani miriyoni gumi nemana emupunga, nematani gumi nerimwe ehuswa. Varimi vanowanzozvipisa mumunda semarara, uko kusiri kungoparadza kukuru kwezviwanikwa, asiwo kunokonzeresa kusvibiswa kwakanyanya kune nharaunda. Naizvozvo, kuziva mashandisirwo ezviwanikwa zvemashanga ndiko kudiwa kwechirongwa chebudiriro yekurima.

1. Kuedza zvinhu uye nzira

1.1 Kuedza zvinhu uye midziyo

Mashanga cellulose, akazvigadzira murabhoritari; JJ～1 mhando yemagetsi musanganisi, Jintan Guowang Experimental Instrument Factory; SHZW2C mhando RS-Pombi yevacuum, Shanghai Pengfu Electromechanical Co., Ltd.; pHS-3C pH mita, Mettler-Toledo Co., Ltd.; DGG-9070A magetsi ekudziya anogara achipisa tembiricha yekuomesa ovheni, Beijing North Lihui Test Instrument Equipment Co., Ltd.; HITACHI-S ~ 3400N kuongorora maikorosikopu erekitironi, Hitachi Instruments; ethanol; sodium hydroxide; chloroacetic acid, nezvimwewo (iyo reagents iri pamusoro iri analytically yakachena).

1.2 Nzira yekuedza

1.2.1 Kugadzirira kwecarboxymethyl cellulose

(1) Nzira yekugadzirira ye carboxymethyl cellulose: Yeresa 2 g ye cellulose mu flask ine mitsipa mitatu, wedzera 2.8 g ye NaOH, 20 mL ye 75% ethanol solution, uye inyoka mualkali mune inogara tembiricha yekugeza mvura pa25.°C kwe80 min. Gadzirai nemuvhenganisi kuti musanganise zvakanaka. Panguva iyi, cellulose inopindirana nealkaline solution kuumba alkali cellulose. Muchikamu cheetherification, wedzera gumi mL ye75% ethanol solution uye 3 g yechloroacetic acid kuflask ine mitsipa mitatu yakabatwa pamusoro, simudza tembiricha kusvika 65-70.° C., uye ita kwemaminitsi makumi matanhatu. Wedzera alkali kechipiri, wobva wawedzera 0.6g NaOH kune iri pamusoro reaction flask kuchengetedza tembiricha iri pa70.°C, uye nguva yekuita ndeye 40min kuti uwane isina Na-CMC (sodium carboxymethylcellulose).

Neutralization uye kugeza: wedzera 1moL·L-1 hydrochloric acid, uye gadzirisa maitiro pane tembiricha yekamuri kusvika pH = 7 ~ 8. Wogeza kaviri ne50% ethanol, wogeza kamwe chete ne95% ethanol, sefa nekusveta, woomesa pa80-90.°C kwemaawa maviri.

(2) Kutemerwa dhigirii rekutsiva sampuli: acidity mita yekumisikidza nzira: Huremu 0.2g (chaiyo kusvika 0.1mg) yeyakacheneswa uye yakaomeswa Na-CMC sampu, inyungudise mu80mL mvura yakarukwa, kurunga nemagetsi kwegumi min, uye gadzirisa. iyo ine acid kana alkali Mushonga wakaunza pH yemushonga kusvika pa8. Wobva waisa mushonga webvunzo nesulfuric acid standard solution mubeaker ine pH meter electrode, woona kuratidzwa kwemamita epH uchitenderera kusvika pH yapera. 3.74. Cherechedza pasi vhoriyamu yesulfuric acid yakajairwa mhinduro inoshandiswa.

1.2.2 Single factor test method

(1) Mhedzisiro yehuwandu hwealkali pachiyero chekutsiva carboxymethyl cellulose: ita alkalization pa25.℃, alkali kunyudzwa kwemaminetsi makumi masere, kunyura mu ethanol solution i75%, kudzora huwandu hwe monochloroacetic acid reagent 3g, etherification tembiricha i65 ~ 70°C, nguva ye etherification yaive maminetsi e100, uye huwandu hwe sodium hydroxide yakachinjirwa bvunzo.

(2) Mhedzisiro yehuwandu hwemhinduro ye ethanol pachiyero chekutsiva carboxymethyl cellulose: huwandu hwealkali yakagadziriswa i3.2g, kunyudzwa kwealkaline mukugezesa kwemvura kunogara kuchipisa pa25.°C ye80min, huwandu hwe ethanol solution i75%, huwandu hwemonochloroacetic acid reagent inodzorwa pa3g, etherification Kupisa kuri 65-70.°C, nguva ye etherification ndeye 100min, uye kusungirirwa kwemhinduro ye ethanol kunoshandurwa pakuedza.

(3) Mhedzisiro yehuwandu hwemonochloroacetic acid pachiyero chekutsiva carboxymethyl cellulose: gadzirisa pa25°C ye alkalization, soak mu alkali kwemaminitsi makumi masere, wedzera 3.2g ye sodium hydroxide kuti iite concentration ye ethanol solution 75%, ether Tembiricha i65 ~ 70°C, nguva ye etherification i100min, uye huwandu hwemonochloroacetic acid hunoshandurwa kuti iedze.

(4) Mhedzisiro yekushisa kwe etherification pachiyero chekutsiva carboxymethyl cellulose: gadzirisa pa25°C ye alkalization, soak mu alkali kwemaminitsi makumi masere, wedzera 3.2g ye sodium hydroxide kuti iite concentration ye ethanol solution 75%, etherification tembiricha Tembiricha iri 65~70℃, iyo etherification nguva ndeye 100min, uye kuedza kunoitwa nekushandura dosage ye monochloroacetic acid.

(5) Mhedzisiro yenguva etherification pachiyero chekutsiviwa kwe carboxymethyl cellulose: yakatarwa pa25°C ye alkalization, yakawedzera 3.2g ye sodium hydroxide, uye yakanyudzwa mu alkali for 80min kuita concentration ye ethanol solution 75%, uye controlled monochlor Muyero weacetic acid reagent i3g, the etherification tembiricha i65~70.°C, uye nguva etherification inoshandurwa kuti iedze.

1.2.3 Chirongwa chekuyedza uye optimization yecarboxymethyl cellulose

Pahwaro hwechinhu chimwe chete chekuedza, quadratic regression orthogonal rotation yakasanganiswa kuedza nezvinhu zvina uye mazinga mashanu akagadzirwa. Zvinhu zvina inguva etherification, etherification tembiricha, huwandu hweNaOH uye huwandu hwemonochloroacetic acid. Kugadziriswa kwedata kunoshandisa SAS8.2 statistical software yekugadzira data, iyo inoratidza hukama pakati pechimwe nechimwe chinofurira chinhu uye dhigirii rekutsiva carboxymethyl cellulose. mutemo wemukati.

1.2.4 SEM yekuongorora nzira

Sampu yehupfu yakaomeswa yakagadziriswa padanho remuenzaniso ine conductive glue, uye mushure mekupfapfaidza goridhe, yakaonekwa uye yakatorwa mifananidzo pasi peHitachi-S-3400N Hitachi scanning electron microscope.

2. Migumisiro uye kuongorora

2.1 Mhedzisiro yechinhu chimwe chete padanho rekutsiva carboxymethyl cellulose

2.1.1 Mhedzisiro yehuwandu hwealkali padanho rekutsiva carboxymethyl cellulose

Apo NaOH3.2g yakawedzerwa kune 2g cellulose, dhigirii yekutsiva yechigadzirwa ndiyo yaive yepamusoro. Nhamba yeNaOH yakaderedzwa, iyo isina kukwana kuumba neutralization yealkaline cellulose uye etherification agent, uye chigadzirwa chine chidimbu chiduku chekugadzirisa uye kuderera kweviscosity. Pane zvinopesana, kana huwandu hweNaOH hwakawandisa, maitiro eparutivi panguva yehydrolysis ye chloroacetic acid inowedzera, kushandiswa kweetherifying agent kuchawedzera, uye viscosity yechigadzirwa ichadererawo.

2.1.2 Mhedzisiro yehuwandu hwemhinduro ye ethanol pachiyero chekutsiva carboxymethyl cellulose

Chikamu chemvura mumushonga we ethanol chiripo mukuita svikiro kunze kwe cellulose, uye chimwe chikamu chiri mu cellulose. Kana mvura yemukati yakakurisa, CMC ichazvimba mumvura kuita jelly panguva ye etherification, zvichikonzera kusaenzana kwakanyanya; kana mvura yemukati iri diki zvakanyanya, kuita kunenge kwakaoma kuenderera nekuda kwekushaikwa kwekuita svikiro. Kazhinji, 80% ethanol ndiyo inonyanya kunyungudutsa.

2.1.3 Mhedzisiro yedosi ye monochloroacetic acid padanho rekutsiva carboxymethyl cellulose

Huwandu hwemonochloroacetic acid uye sodium hydroxide ndeye theoretically 1: 2, asi kuti ufambise maitiro kune kutungamira kwekugadzira CMC, ita shuwa kuti pane yakakodzera hwaro hwemahara muhurongwa hwekuita, kuitira kuti carboxymethylation ienderere mberi zvakanaka. Nokuda kwechikonzero ichi, nzira yekuwedzera alkali inogamuchirwa, kureva, iyo molar ratio yeasidhi uye alkali zvinhu ndeye 1: 2.2.

2.1.4 Mhedzisiro yekushisa kwe etherification pane dhigirii yekutsiva carboxymethyl cellulose

Kukwirisa tembiricha ye etherification, ndiko kukurumidza kuita mwero, asi maitiro epadivi anokwidziridzwawo. Kubva pakuona kwekemikari chiyero, kukwira kwekushisa hakuna kunaka pakuumbwa kweCMC, asi kana tembiricha yakadzikira, chiyero chekuita chinononoka uye chiyero chekushandisa cheetherifying agent chakaderera. Zvinogona kuonekwa kuti yakanyanya tembiricha ye etherification i70°C.

2.1.5 Mhedzisiro yenguva etherification pane dhigirii rekutsiva carboxymethyl cellulose

Nekuwedzera kwenguva ye etherification, dhigirii rekutsiva CMC rinowedzera, uye kukurumidza kwekuita kunokwidziridzwa, asi mushure meimwe nguva, maitiro epadivi anowedzera uye dhigirii rekutsiva rinodzikira. Kana nguva ye etherification iri 100min, dhigirii rekutsinhanisa rinonyanya.

2.2 Orthogonal bvunzo mhedzisiro uye kuongororwa kwecarboxymethyl mapoka

Zvinogona kuonekwa kubva pane tafura yekuongorora mutsauko kuti muchinhu chekutanga, zvinhu zvina zvenguva ye etherification, etherification tembiricha, huwandu hweNaOH uye huwandu hwemonochloroacetic acid zvine simba rakanyanya padanho rekutsiva carboxymethyl cellulose (p. <0.01). Pakati pezvinhu zvekudyidzana, zvinhu zvekudyidzana zvenguva ye etherification uye huwandu hwemonochloroacetic acid, uye zvinhu zvekudyidzana kwekushisa kwe etherification uye huwandu hwemonochloroacetic acid zvakave nemhedzisiro yakakosha padanho rekutsiva carboxymethyl cellulose (p <0.01). Kurongeka kwekupesvedzera kwezvinhu zvakasiyana-siyana pachiyero chekutsiva carboxymethyl cellulose yaive: etherification tembiricha> kuwanda kwe monochloroacetic acid> etherification nguva> kuwanda kweNaOH.

Mushure mekuongororwa kwemhedzisiro yebvunzo yequadratic regression orthogonal rotation musanganiswa dhizaini, zvinogona kutariswa kuti iyo yakakwana maitiro ekugadzirisa carboxymethylation gadziriso ndeiyi: etherification nguva 100min, etherification tembiricha 70.℃, NaOH dosage 3.2g uye monochloroacetic acid Muyero ndeye 3.0g, uye dhigirii yakawanda yekutsiva ndeye 0.53.

2.3 Microscopic performance performance

Iyo yepamusoro morphology ye cellulose, carboxymethyl cellulose uye muchinjika-yakabatana carboxymethyl cellulose particles yakaongororwa nekuongorora maelectron microscopy. Iyo cellulose inokura muchimiro chemitsetse ine nzvimbo yakatsetseka; mupendero wecarboxymethyl cellulose wakashata kupfuura weiyo yakabviswa cellulose, uye iyo cavity chimiro inowedzera uye vhoriyamu inova yakakura. Izvi zvinodaro nekuti chimiro chebundle chinova chakakura nekuda kwekuzvimba kwecarboxymethyl cellulose.

3. Mhedziso

3.1 Kugadzirira kwecarboxymethyl etherified cellulose Kurongeka kwekukosha kwezvinhu zvina zvinokanganisa dhigirii yekutsiva cellulose ndeiyi: etherification tembiricha > monochloroacetic acid dosage > etherification time > NaOH dosage. Iyo yakanyanya kunaka maitiro ekugadzirisa carboxymethylation ndeye etherification nguva 100min, etherification tembiricha 70.℃, NaOH dosage 3.2g, monochloroacetic acid dosage 3.0g, uye yakanyanya kutsiva dhigirii 0.53.

3.2 Iwo akanakisa tekinoroji mamiriro ecarboxymethylation shanduko ndeaya: etherification nguva 100min, etherification tembiricha 70.℃, NaOH dosage 3.2g, monochloroacetic acid dosage 3.0g, yakanyanya kutsiva dhigirii 0.53.