CMC Cellulose iyo Qaab-dhismeedkeeda

Isticmaalka cellulose caws sida walxo ceeriin ah, waxaa lagu beddelay etherification. Iyada oo loo marayo hal arrin iyo tijaabada wareegga, xaaladaha ugu fiican ee diyaarinta karboxymethyl cellulose ayaa lagu go'aamiyay inay noqdaan: waqtiga etherification 100min, heerkulka etherification 70℃, Qiyaasta NaOH 3.2g iyo monochloroacetic acid qiyaasta 3.0g, beddelka ugu badan ee darajadu waa 0.53.

Erayada muhiimka ah: CMCcellulose; monochloroacetic acid; etherification; wax ka beddel

Carboxymethyl cellulosewaa ether-ka cellulose-ka ugu badan ee la soo saaro oo la iibiyo. Waxaa si weyn loogu isticmaalaa saabuunta, cuntada, daawada cadayga, dunta, daabacaadda iyo rinjiyeynta, waraaqaha samaynta, Batroolka, macdanta, daawaynta, dhoobada, qaybaha elektarooniga ah, cinjirka, Rinjiga, sunta cayayaanka, waxyaalaha la isku qurxiyo, maqaar, baco iyo saliid qodista, iwm. sida "Monosodium glutamate warshadaha". Carboxymethyl cellulose waa derivative cellulose ether ah oo biyo-milmi kara oo la helay iyadoo kiimiko ahaan wax looga beddelayo cellulose dabiiciga ah. Cellulose, oo ah alaabta ceeriin ee ugu weyn ee soo saarista karboxymethyl cellulose, waa mid ka mid ah kheyraadka dabiiciga ah ee dib loo cusboonaysiin karo ee ugu badan ee dhulka, iyada oo wax soo saarka sanadlaha ah boqolaal balaayiin tan ah. dalkaygu waa waddan beeraley ah oo baaxad weyn, kana mid ah dalalka ugu kheyraadka badan ee cawska. Cawsku waxay had iyo jeer ahaa mid ka mid ah shidaalka ugu muhiimsan ee ay ku nool yihiin dadka deggan miyiga. Khayraadkaas oo aan si caqli-gal ah loo horumarin muddo dheer, wax ka yar 2% qashinka beeraha iyo kaymaha sida cawska ayaa laga isticmaalaa adduunka sannad kasta. Bariiska waa dalagga dhaqaalaha ugu weyn ee Gobolka Heilongjiang, oo leh dhul beereedka in ka badan 2 milyan hm2, wax soo saarka sanadlaha ah 14 milyan oo tan oo bariis ah, iyo 11 milyan oo tan oo caws ah. Beeralayda guud ahaan waxay si toos ah ugu gubaan beerta sida qashinka, taas oo aan ahayn oo kaliya qashinka weyn ee kheyraadka dabiiciga ah, laakiin sidoo kale waxay keentaa wasakh halis ah deegaanka. Sidaa darteed, xaqiijinta ka faa'iidaysiga kheyraadka cawsku waa baahida loo qabo istaraatiijiyad horumarineed oo waara ee beeralayda.

1. Qalabka tijaabada iyo hababka

1.1 Qalabka tijaabada ah iyo qalabka

cellulose caws, is-dhigay shaybaarka; JJ～1 nooc isku-darka korantada, Warshada Qalabka Tijaabada ee Jintan Guowang; SHZW2C nooca RS-Bamka faakuumka ah, Shanghai Pengfu Electromechanical Co., Ltd.; pHS-3C mitirka pH, Mettler-Toledo Co., Ltd.; DGG-9070A kululaynta korontada foornada heerkulka joogtada ah, Beijing North Lihui Test Instrument Equipment Co., Ltd .; HITACHI-S ~ 3400N mikroskoob ee elektarooniga ah, Qalabka Hitachi; ethanol; sodium hydroxide; chloroacetic acid, iwm. (reagen-yaasha sare waa falanqeyn ahaan saafi ah).

1.2 Habka tijaabada ah

1.2.1 Diyaarinta carboxymethyl cellulose

(1) Habka diyaarinta ee carboxymethyl cellulose: Miisaanka 2 g of cellulose galay weel saddex-qoor leh, ku dar 2.8 g of NaOH, 20 mL of 75% ethanol xal, iyo qooyay alkali in qubeyska heerkulka joogto ah biyaha at 25°C ilaa 80 daqiiqo. Ku walaaq qaseeyaha si aad si fiican isugu darsato. Inta lagu jiro habkan, cellulose waxay la falgashaa xalalka alkaline si ay u sameyso alkali cellulose. Marxaladda etherification, ku dar 10 ml oo ah 75% ethanol xal ah iyo 3 g oo ah chloroacetic acid weelka saddexda luqun ee kor ku xusan, kor u qaad heerkulka 65-70° C., oo ka jawaab 60 daqiiqo. Ku dar alkali mar labaad, ka dibna ku dar 0.6g NaOH weelka falcelinta ee kore si aad heerkulka ugu ilaaliso 70°C, iyo wakhtiga falcelintu waa 40min si loo helo cayriin Na-CMC (sodium carboxymethylcellulose).

Dhexdhexaadinta iyo dhaqidda: ku dar 1mL·L-1 hydrochloric acid, oo ka takhalus falcelinta heerkulka qolka ilaa pH = 7 ~ 8. Ka dib laba jeer ku maydh 50% ethanol, ka dibna hal mar ku maydh 95% ethanol, ku sifee nuugista, oo ku qalaji 80-90°C ilaa 2 saacadood.

(2) Go'aaminta heerka beddelka muunadda: Habka go'aaminta mitirka aysiidhka: Miisaanka 0.2g (sax ah ilaa 0.1mg) ee muunadda Na-CMC ee la safeeyey oo la qalajiyey, ku milmi 80mL biyo nadiif ah, walaaq koronto 10min, oo hagaaji waxay la socotaa aashito ama alkali Xalku wuxuu keenay pH ee xalka ilaa 8. Ka dibna titrate xalka tijaabada leh sulfuric acid xal heerka beaker ku qalabaysan mitir pH electrode ah, oo fiirso tilmaanta pH meter inta titrating ilaa pH waa. 3.74. U fiirso mugga xalalka sulfuric acid ee la isticmaalay.

1.2.2 Habka tijaabada halbeegga ah

(1) Saamaynta qaddarka alkali ee heerka beddelka karboxymethyl cellulose: samee alkalization at 25℃, immersion alkali 80 daqiiqo, fiirsashada ee xalka ethanol waa 75%, xakamee qadarka monochloroacetic acid reagent 3g, heerkulka etherification waa 65 ~ 70°C, wakhtiga etherification wuxuu ahaa 100 daqiiqo, iyo qadarka sodium hydroxide ayaa loo bedelay baaritaanka.

(2) Saamaynta fiirsashada ee xalka ethanol ee heerka beddelka carboxymethyl cellulose: qadarka alkali go'an waa 3.2g, immersion alkaline qubeyska heerkulka joogtada ah ee biyaha at 25°C ee 80min, xoojinta xalka ethanol waa 75%, qadarka monochloroacetic acid reagent waxaa lagu xakameynayaa 3g, etherification Heerkulka waa 65-70°C, wakhtiga etherification waa 100min, iyo xoojinta xalka ethanol ayaa loo beddelay tijaabada.

(3) Saamaynta qaddarka monochloroacetic acid ee heerka beddelka karboxymethyl cellulose: hagaaji 25°C ee alkalization, qooyay alkali 80 daqiiqo, ku dar 3.2g of sodium hydroxide si ay u sameeyaan diirada ethanol xal 75%, ether Heerkulka waa 65 ~ 70°C, wakhtiga etherification waa 100min, iyo qadarka monochloroacetic acid waa la bedelay si tijaabo ah.

(4) Saamaynta heerkulka etherification ee heerka beddelka karboxymethyl cellulose: hagaajin at 25°C ee alkalization, qooyay alkali 80 daqiiqo, ku dar 3.2g of sodium hydroxide si ay u fiirsashada of xal ethanol 75%, heerkulka etherification Heerkulka waa 65 ~ 70℃, waqtiga etherification waa 100min, iyo tijaabada waxaa lagu fuliyaa iyadoo la bedelayo qiyaasta monochloroacetic acid.

(5) Saamaynta wakhtiga etherification ee heerka beddelka karboxymethyl cellulose: go'an 25°C ee alkalization, lagu daray 3.2g of sodium hydroxide, oo lagu qooyay alkali for 80min si ay u sameeyaan fiirsashada ee xal ethanol 75%, iyo monochlor la xakameeyey Qiyaasta reagent acetic acid waa 3g, heerkulka etherification waa 65 ~ 70°C, iyo wakhtiga etherification ayaa loo beddelay tijaabada.

1.2.3 Qorshaha tijaabada iyo hagaajinta karboxymethyl cellulose

Iyada oo ku saleysan tijaabada hal-abuurka ah, wareegtada dib-u-celinta quadratic-ka ah ee isku-dhafka ah ee tijaabinta afar arrimood iyo shan heer ayaa la qorsheeyay. Afarta arrimood waa wakhtiga etherification, heerkulka etherification, qadarka NaOH iyo qadarka monochloroacetic acid. Habaynta xogta waxay isticmaashaa SAS8.2 software xisaabeedka habaynta xogta, taas oo muujinaysa xidhiidhka ka dhexeeya arrin kasta oo saamaynaysa iyo heerka beddelka karboxymethyl cellulose. sharciga gudaha.

1.2.4 Habka falanqaynta SEM

Muunadda budada qallalan ayaa lagu hagaajiyay marxaladda muunada iyadoo leh koollo wax-qabad ah, ka dib markii vacuum lagu buufiyo dahab, waxaa lagu arkay oo lagu sawiray Mikroskoob elektaroonig ah oo Hitachi-S-3400N Hitachi ah.

2. Natiijooyinka iyo falanqaynta

2.1 Saamaynta hal arrin ee heerka beddelka karboxymethyl cellulose

2.1.1 Saamaynta qaddarka alkali ee heerka beddelka karboxymethyl cellulose

Markii NaOH3.2g lagu daray 2g cellulose, heerka beddelka alaabada ayaa ahayd kan ugu sarreeya. Qadarka NaOH waa la dhimay, taas oo aan ku filnayn in la sameeyo dhexdhexaadinta cellulose alkaline iyo wakiilka etherification, iyo alaabtu waxay leedahay heer yar oo beddelaad ah iyo muuqaal hoose. Taas bedelkeeda, haddii qadarka NaOH uu aad u badan yahay, falcelinta dhinaca inta lagu jiro hydrolysis of chloroacetic acid ayaa kordhin doona, isticmaalka wakiilka etherifying ayaa kordhi doona, iyo viscosity alaabta ayaa sidoo kale hoos u dhigi doonta.

2.1.2 Saamaynta fiirsashada ee xalka ethanol ee heerka beddelka carboxymethyl cellulose

Qayb ka mid ah biyaha ku jira xalka ethanol waxay ku jiraan dhexdhexaadinta falcelinta ka baxsan cellulose, iyo qaybta kale waxay ku jirtaa cellulose. Haddii biyaha ku jira ay aad u weyn yihiin, CMC waxay ku barari doontaa biyaha si ay u sameeyaan jelly inta lagu jiro etherification, taasoo keentay falcelin aan sinnayn; haddii biyaha ku jira ay aad u yar yihiin, falcelinta way adkaan doontaa in la sii wado sababtoo ah la'aanta dhexdhexaadinta falcelinta. Guud ahaan, 80% ethanol waa dareeraha ugu habboon.

2.1.3 Saamaynta qiyaasta monochloroacetic acid ee heerka beddelka carboxymethyl cellulose

Qadarka monochloroacetic acid iyo sodium hydroxide waa aragti ahaan 1: 2, laakiin si loo dhaqaajiyo falcelinta jihada soo saarista CMC, hubi in ay jirto saldhig bilaash ah oo ku habboon nidaamka falcelinta, si karboxymethylation ay u socoto si habsami leh. Sababtan awgeed, habka alkali ee xad-dhaafka ah ayaa la qaataa, taas oo ah, saamiga molar ee acid iyo walxaha alkali waa 1: 2.2.

2.1.4 Saamaynta heerkulka etherification ee heerka beddelka carboxymethyl cellulose

Markasta oo uu sarreeyo heerkulka etherification, si dhakhso ah ayuu u kordhiyaa heerka falcelinta, laakiin falcelinta dhinacyadu sidoo kale waa la dedejiyaa. Marka laga eego dhinaca dheelitirka kiimikada, heerkulka kor u kaca waa mid aan fiicnayn samaynta CMC, laakiin haddii heerkulku aad u hooseeyo, heerka falcelintu waa gaabis iyo heerka isticmaalka ee wakiilka etherifying waa hooseeyaa. Waxaa la arki karaa in heerkulka ugu fiican ee etherification uu yahay 70°C.

2.1.5 Saamaynta wakhtiga etherification ee heerka beddelka karboxymethyl cellulose

Kordhinta wakhtiga etherification, heerka beddelka CMC wuu kordhiyaa, xawaaraha falcelinta waa la dedejiyaa, laakiin wakhti go'an ka dib, falcelinta dhinacyadu way kordhaan oo heerka beddelka ayaa hoos u dhacaya. Marka wakhtiga etherification uu yahay 100min, heerka bedelku waa ugu badnaan.

2.2 Natiijooyinka baaritaanka orthogonal iyo falanqaynta kooxaha carboxymethyl

Waxaa laga arki karaa miiska falanqaynta kala duwanaansho in sheyga aasaasiga ah, afarta arrimood ee wakhtiga etherification, heerkulka etherification, qadarka NaOH iyo qadarka monochloroacetic acid ay saameyn aad u weyn ku leedahay heerka beddelka karboxymethyl cellulose (p) <0.01) Waxyaabaha isdhexgalka, walxaha isdhexgalka ee wakhtiga etherification iyo qadarka monochloroacetic acid, iyo walxaha isdhexgalka ee heerkulka etherification iyo qadarka monochloroacetic acid ayaa saameyn aad u weyn ku yeeshay heerka beddelka karboxymethyl cellulose (p <0.01). Nidaamka saameynta arrimo kala duwan oo ku saabsan heerka beddelka karboxymethyl cellulose wuxuu ahaa: heerkulka etherification> qaddarka monochloroacetic acid> wakhtiga etherification> qaddarka NaOH.

Ka dib markii la falanqeeyo natiijooyinka imtixaanka ee naqshadeynta isku-dhafka wareegga wareegga wareegga afar-geesoodka ah, waxaa la go'aamin karaa in shuruudaha habka ugu wanaagsan ee wax-ka-beddelka karboxymethylation ay yihiin: waqtiga etherification 100min, heerkulka etherification 70℃, NaOH qiyaasta 3.2g iyo monochloroacetic acid Qiyaastu waa 3.0g, heerka ugu badan ee beddelkuna waa 0.53.

2.3 Tilmaamaha waxqabadka microscopic

Qaab-dhismeedka dusha sare ee cellulose, karboxymethyl cellulose iyo qaybaha karboxymethyl cellulose-ku-xiran ee isku-dhafan ayaa lagu bartay iyadoo la baarayo mikroskoobyada elektarooniga ah. Cellulose waxay ku koraan qaab xariijimo leh oo siman; cidhifka cellulose karboxymethyl waa ka qallafsan yahay kan cellulose-ka la soo saaray, iyo qaab-dhismeedka dalool kordho iyo mugga weyn yahay. Tani waa sababta oo ah qaab-dhismeedka xidhmo ayaa noqda mid weyn sababtoo ah bararka karboxymethyl cellulose.

3. Gabagabo

3.1 Diyaarinta karboxymethyl etherified cellulose Nidaamka muhiimka ah ee afarta arrimood ee saameeya heerka beddelka cellulose waa: heerkulka etherification> qiyaasta monochloroacetic acid> Waqtiga etherification> Qiyaasta NaOH. Xaaladaha habka ugu fiican ee wax ka beddelka karboxymethylation waa wakhtiga etherification 100min, heerkulka etherification 70℃, Qiyaasta NaOH 3.2g, qiyaasta aashitada monochloroacetic 3.0g, iyo heerka ugu badan ee beddelka 0.53.

3.2 Xaaladaha tignoolajiyada ugu fiican ee wax ka beddelka karboxymethylation waa: wakhtiga etherification 100min, heerkulka etherification 70℃, Qiyaasta NaOH 3.2g, qiyaasta aashitada monochloroacetic 3.0g, heerka beddelka ugu badan 0.53.