第34卷第4期太原理工Vol 34 No 42003年7月JOURNAL OF TAIYUAN UNIVERSITY OF TECHNOLOGYJuly 2003文章編號(hào):1007-9432(2003)04-0449-03丙烯酸鹽和丙烯酰胺共聚物的制備李愛秀太原理工大學(xué)測試中心,山西太原030024)摘要:以丙烯酸為原料,加入少量丙烯酰胺和礦物鹽,用偶氮二異丁腈為引發(fā)劑速聚而成種新型增稠劑。并將其性能和印染效罘與藻朊酸鈉作了對(duì)比。鮚釆表明,該増稠劑増稠效果與藻朊酸鈉相當(dāng),并用紅外光譜驗(yàn)證了產(chǎn)品的結(jié)構(gòu)。關(guān)鍵詞:丙烯酸;丙烯酰胺;偶氪二異丁腈;藻朊酸鈉;引發(fā)劑中圖分類號(hào):TQ203;TQ610.4文獻(xiàn)標(biāo)識(shí)碼:A目前國內(nèi)外多數(shù)紡織印染廠用藻朊酸鈉作活性反應(yīng)液倒入盛有引發(fā)劑溶液的塑料速聚反應(yīng)器中染料的糊料,但是藻朊酸鈉是一種天然的增稠劑,資進(jìn)行速聚得白色孔性固體產(chǎn)物,在105℃烘干并粉源奇缺,價(jià)格昂貴,所以開發(fā)它的代用品是勢(shì)在必碎。行。許多國家正在研究開發(fā)藻朊酸鈉的代用品。日本的KoKo, Shigetoshi等所申請(qǐng)的專利是用羧甲2結(jié)果與討論基淀粉纖維素混合物的堿金屬鹽來代替藻朊酸鈉2.1工藝的選擇網(wǎng)印棉織物。 Ortega Theresa m申請(qǐng)的歐洲專利合成工藝主要選擇引發(fā)劑及配料比。引發(fā)劑是用一種雜環(huán)化合物和水溶性的多糖與藻朊酸鈉混有:高錳酸鉀檸檬酸引發(fā)體系,過硫酸鉀引發(fā)體系,合印染棉織品與地毯。埃及的A. Hebeish等先后偶氮二異丁腈的引發(fā)體系。最后選擇最佳的一種偶發(fā)表了幾篇論文2-,研究以聚丙烯酸淀粉組成物氮二異丁腈的引發(fā)體系,該引發(fā)劑能在低沸點(diǎn)有機(jī)代替藻朊酸鈉,印染物的著色強(qiáng)度、水洗牢度和干磨溶劑中迅速溶解,而且速聚速度快產(chǎn)量高。合成工牢度等指標(biāo)不穩(wěn)定,其主要原因是未接枝的淀粉在藝見表1起作用。本文研究的是一種丙烯酸與少量丙烯酰胺表1合成工藝配方及少量礦物鹽的共聚物,其增稠效果與藻朊酸鈉相當(dāng),優(yōu)點(diǎn)是價(jià)格低,抗菌性好,易洗除,著色強(qiáng)調(diào)高會(huì)入原料丙烯酸丙烯酰膠發(fā)劑礦物鹽1物鹽2碳酸堿水滲透性好。實(shí)驗(yàn)部分1.1原料與儀器原料:丙烯酸(工業(yè)級(jí)),碳酸鉀(工業(yè)級(jí))丙烯[注:+”為合成時(shí)所加人的原料,一”表示合成時(shí)沒有該原料酰胺(工業(yè)級(jí)),偶氮二異丁腈(工業(yè)級(jí)),高錳酸鉀(CP),檸檬酸(CP),過硫酸鉀(CP),藻朊酸鈉(工業(yè)從表1知,配方Ⅰ粘度低厚度不夠;配方Ⅱ加入級(jí))。設(shè)備:塑料速聚反應(yīng)器;電動(dòng)攪拌器;升降臺(tái)礦物鹽1后,厚度增加,但粘度仍小;配方Ⅲ加入礦電熱套;水浴鍋;ND旋轉(zhuǎn)式粘度計(jì);FTIR1730紅物鹽2后厚度增加不如礦物鹽1明顯;配方N加入外光譜儀(美國PE公司)丙烯酰胺后粘度增大且流線性好但厚度差;配方V1.2合成方法克服中國煤化工選擇配方Ⅴ進(jìn)行平行在500mL的不銹鋼杯中安裝電動(dòng)攪拌器,加試驗(yàn)CNMHG入一定量水,同時(shí)加入一定量堿,直到堿全部溶解。2.2試印染結(jié)果然后慢慢加入丙烯酸和礦物鹽,pH=6~7,最后將產(chǎn)品試印染小樣試驗(yàn)在山西省紡織印染廠進(jìn)收稿早請(qǐng)數(shù)(56-),女、山西忻州人,高級(jí)工程師,主要從事淀粉深加工及儀器分析研究150太原理工大學(xué)學(xué)報(bào)第34卷行,并與海漿試印染結(jié)果進(jìn)行比較,見表2.從著色把產(chǎn)品配制成不同質(zhì)量濃度來測定粘度。由圖強(qiáng)度、手感的柔軟度、皂煮褪色、皂煮白沾、濕燙白1看岀,粘度隨質(zhì)量濃度的增加而增加沾、濕磨、干磨等牢度試驗(yàn)與海漿進(jìn)行了對(duì)比,各項(xiàng)在聚合反應(yīng)中控制丙烯酰胺的加入量然后測定性能指標(biāo)均接近,達(dá)到或超過海漿。特別是皂煮褪粘度。由圖2發(fā)現(xiàn)丙烯酰胺的加入量與粘度有很大色、著色等指標(biāo)均優(yōu)于海漿。關(guān)系,隨丙烯酰胺的加人量增加而增加表2產(chǎn)品與海漿試印染結(jié)果比較由圖3可見,海漿粘度隨轉(zhuǎn)動(dòng)速度增加而迅速性能!煮褪色皂煮白沾濕燙白沾干磨下降。海漿由圖4發(fā)現(xiàn),產(chǎn)品粘度和海漿粘度相似,隨轉(zhuǎn)動(dòng)2柔軟速度的增大也迅速下降。2.4產(chǎn)品結(jié)構(gòu)分析2.3產(chǎn)品的粘度6結(jié)構(gòu)分析主要靠IR光譜來驗(yàn)證結(jié)構(gòu),如圖5,印染效果的好壞與產(chǎn)品的粘度有很大的關(guān)系圖6所示。所以對(duì)粘度進(jìn)行了比較詳細(xì)的研究。如圖1~圖4420051.01.520253.0產(chǎn)品質(zhì)量濃度/gL內(nèi)烯酰胺質(zhì)量濃度/gL1質(zhì)量濃度與粘度的關(guān)系圖2丙烯酰胺加入量與粘度的關(guān)系2.430圖3海漿粘度與轉(zhuǎn)動(dòng)速度的關(guān)系圖4產(chǎn)品粘度與轉(zhuǎn)動(dòng)速度的關(guān)系400030002000400030002000波數(shù)/cm圖5丙烯酸的IR光譜圖圖6產(chǎn)品的IR光譜圖圖5為丙烯酸的R光諧圖。從圖5可以看到.圖6V山中國煤化工而增加了飽和烴亞甲峰1(3423cm-1)為-OH,CH=CH2氧氫鍵和基峰CNMHGH-碳?xì)渖炜s振動(dòng)峰烯烴碳?xì)滏I的伸縮振動(dòng)峰,峰2(lτσ3cm-)為C≡峰3峰Δ為聚丙烯酸鹽的特征吸收峰,峰3(1568O的伸縮振動(dòng)峰,峰3(1636cm-1)為C=C的伸縮cm-1)為一CO0一的反對(duì)稱的伸縮振動(dòng),峰4(1403振動(dòng)峰,峰4,峰5,峰6為一CH=CH端基烯面內(nèi)cm-1)為一COO一的對(duì)稱的伸縮振動(dòng),所以確定該與面外彎和、玀。圖6為產(chǎn)品的IR光譜圖。從產(chǎn)品的結(jié)構(gòu)主要是聚丙烯酸鹽第4期李愛秀:丙烯酸鹽和丙烯酰胺共聚物的制備451廢水排放,因而產(chǎn)品成本比較低。所得產(chǎn)品增稠效3結(jié)論果好,物理與化學(xué)性質(zhì)穩(wěn)定,流動(dòng)性好,可全部或部本研究所選用的速聚工藝的優(yōu)點(diǎn)是:所用的生分代替藻朊酸鈉作為活性染料的增稠劑產(chǎn)設(shè)備少,生產(chǎn)周期短,能耗低,產(chǎn)率高且無廢料和參考文獻(xiàn)[1 Koko. Shigetoshi, et al. Printing Pastes Containing Carboxylmethylated Starch-cellulose Mixtures[P]. JP 0297281990-03-30[2 Bayazeed A, Elzairy M R. Hebeish A, Synthesis and application of new thickeners[]. Starch/ Starke. 1989, 41(6): 233-236[3 Hebeish A. Elrafie M H, Higazy A, et aL. Polyid )Starch Composites. A key For Improving Sizeability and De-sizeability of Starch from Cotton Textiles[J]. Starch/Starke,1992.44(3):101-107[4 Hebeish A, Elzairy M H, Elrafie M H, et al. Poly( acrylic acid Starch Composite as a Substitute for Sodium Alginate inPrinting Cotton Fabrics With Reactive Dyes[J]. Starch/Starke, 1991. 43(3):98-102[5]候毓汾,程侶伯.活性染料[M].北京:化學(xué)工業(yè)出版社,1991:516-528[6]虞志光.高聚物分子量及其分布的測定[M].上海:上?？茖W(xué)技術(shù)出版社,1984:21-577]王正熙.聚合物的紅外光譜分析和鑒定[M].成都:四川大學(xué)出版社,1989:154-168Preparation of the copolymer of Acrylic Salt and acrylamideLI Ai-xiuCenter of Measuring and Testing of TUT, Taiyuan 030024 China)Abstract: This work mainly studies a kind of novel thickener with acrylicacid as raw materialand azobisisobutyronitrile as initiator, which produced by joining a small quantity of acrylamideand mineral salts and rapidly aggregating Its performances and effect for printing and dyeing arecompared with those of sodium alginate, and its thickening effect is found to be equal to that ofsodium alginate. The structure of the product is studied using IR spectrumKey words: acrylic acid; acrylamide; azobisisobutyronitrile; sodium alginate; initiato(編輯:張紅霞)部部部部當(dāng)當(dāng)部部部當(dāng)部當(dāng)部當(dāng)當(dāng)部當(dāng)部當(dāng)部部部部部當(dāng)部部部部當(dāng)部當(dāng)部當(dāng)當(dāng)部當(dāng)部當(dāng)當(dāng)當(dāng)部當(dāng)部(上接第448頁)Study on the dimethoxyacetic Acid Methyl Ester SynthesisCHANG Hong-hong, WEI Wen-long, LIU Qiang, LI Yan-wei( College of Chemical Engineering Technology of TUT, Taiyuan 030024 China)Abstract: A new process has been developed to synthesize dimethoxyacetic acid methyl esterfrom 50% solution of glyoxylic acid and methyl orthoformate through catalyzing by concentratedsulfuric acid. On the basis of observing and studying synthetic process conditions, the reactionconditions have been optimized by orthogonal experimet中國煤化工n rate was ud to92. 16% of dimethoxyacetic acid methyl ester.CNMHGKey words: glyoxylic acid; methyl orthoformate; ortIdimethoxyacetic acid methyl ester(編輯:張紅霞)