反相乳液法制备水溶性阳离子共聚物研究
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摘要
反相乳液聚合具有聚合速度快,产物固含量高,分子量大,散热快等优点。反相乳液聚合法广泛地应用于纺织工业中的粘合剂、增稠剂,石油及造纸工业中的絮凝剂、增稠剂和增强剂,以及涂料、医药等行业。
本文以丙烯酰胺(AM)为主要原料,分别与甲基丙烯酰氧乙基三甲基氯化铵(DMC)、二甲基二烯丙基氯化铵(DMDAAC)、二烯丙基胺(DA)、2-丙烯酰胺-2-甲基丙磺酸(AMPS)等单体进行反相乳液聚合,分别合成了AM/DMC共聚物、AM/DMDAAC共聚物、AM/DA共聚物、AM/AMPS/DMDAAC三元共聚物,并对四种不同结构特征的阳离子聚合物进行表征及性质测定。
(1)对于AM/DMC共聚物体系,采用过硫酸钾-四甲基乙二胺(KPS-TMEDA)为引发剂,Span系列乳化剂山梨糖醇酐油酸酯(Span-80)与OP系列乳化剂辛烷基酚聚氯乙烯醚(OP-10)复配作为复合乳化体系,选择环己烷为油相,合成了季铵型的P(AM/DMC)共聚物。通过实验,对反应条件进行了深入研究,确定了最佳反应温度、油水比、引发剂用量、乳化剂用量、单体浓度、单体配比,并对合成的共聚物进行了表征。将P(AM/DMC)共聚物的红外光谱与PAM的红外光谱进行了比较,发现了P(AM/DMC)共聚物的特征吸收峰;用元素分析对P(AM/DMC)共聚物的组成进行了测定;将不同单体配比的P(AM/DMC)共聚物进行了热失重分析;对P(AM/DMC)共聚物进行了核磁共振氢谱表征,谱图中的吸收峰与共聚物分子式基本吻合。以上表征说明了AM与DMC发生了很好的共聚。
(2)对于AM/DMDAAC共聚物体系,采用2-2'-偶氮(2-甲基丙基脒)二盐酸盐(AIBA)为引发剂,Span-80/OP-10为复合乳化剂,选择环己烷为油相,合成了季铵型P(AM/DMDAAC)共聚物。讨论了反应温度、引发剂浓度、单体浓度、单体配比对产物特性黏度和产率的影响。利用红外光谱、元素分析、热失重等检测手段对合成的共聚物P(AM/DMDAAC)进行了表征,结果证明加入的单体进行了很好的共聚。
(3)对于AM/DA共聚物体系,以AIBA为引发剂,Span-80/OP-10为复合乳化剂,环己烷为油相,制备了仲胺型的P(AM/DA)阳离子聚合物。反应前用盐酸中和单体DA,以防止其发生链转移。固定其它反应条件不变,用乌氏粘度计测定了在不同引发剂浓度下产物P(AM/DA)的特性黏度及产率;以此类推,测定了在不同单体浓度、单体配比条件下产物P(AM/DA)的特性黏度及产率。由此得出了制备P(AM/DA)共聚物的最佳反应条件。对产物P(AM/DA)做了红外光谱、元素分析、热失重、核磁共振氢谱、静态激光光散射表征,结果证明AM与DA发生了很好的共聚。对三种不同单体配比的共聚物溶液进行了酸碱滴定,滴定结果与元素分析结果基本吻合。
(4)对于AM/AMPS/DMDAAC共聚物体系,采用引发剂AIBA,复合乳化剂Span-80/OP-10,选择环己烷为油相,合成了两性结构的P(AM/AMPS/DMDAAC)三元共聚物。通过实验,研究了引发剂用量、单体浓度、单体配比对产物特性黏度和产率的影响。对产物P(AM/AMPS/DMDAAC)进行了红外光谱、元素分析、热失重表征,结果说明了AM与AMPS及DMDAAC发生了很好的共聚。
The inverse emulsion polymerization has the merit of high polymerization velocity、high product solidity、high molecular weight、moderate reaction conditions and so on.The inverse emulsion polymerization has widely application in adhesive、thickening agent in textile industry、flocculating agent、thickening agent、intensifier in petroleum and paper making、dope、medicine and so on.
In this paper,four kinds of cationic copolymer were synthesized by the inverse emulsion polymerization using monomers such as acrylamide(AM), methacryloxyethyl trimethyl ammonium chloride(DMC),diallyldimethylammonium chloride(DMDAAC),diallylamine(DA),2-Acrylamido-2-Methylpropane Sulfonic Acid(AMPS).The experimental conditions were studied detailedly to obtain optimum reaction conditions,including of temperature,the content of initiators ratio and content of different monomers,the content of emulsifier.
For AM/DMC copolymer system,potassium persulfate tetramethylethylenediamine(KPS-TMEDA) was used as initiator;Emulsifier sorbitan monooleate(Span-80)/Polyoxyethylene octylphenol ether(OP-10) was used as compound emulsifier;Cyclohexane was choosed as oil phase.Through experiment, the reaction conditions were studied and the best temperature、oil-water ratio、initiator concentration、emulsifier concentration、monomer concentration and monomer ratio were determined.The IR spectra of poly(AM-co-DMC) and PAM were compared, the characteristic peak of poly(AM-co-DMC) was discovered.The composition of poly(AM-co-DMC)was obtained by Elementary analysis.The copolymers poly(AM-co-DMC) of different monomer ratio were made TG analysis;Nuclear magnetic resonance of Poly(AM-co-DMC) showed that the absorption peaks were fundamentally accordant with its structure.The above representation described that AM and DMC have copolymerised.
For AM/DMDAAC copolymer system,2,2' -Azobis(2-methylpropionamide) dihydrochloride(AIBA) was used as initiator,Span80/OP-10 was used as emulsifier, Cyclohexane was choosed as oil phase.The copolymer P(AM/DMDAAC) was synthesized.The influence of temperature、initiator concentration、monomer concentration and monomer ratio on the product's viscosity and yield was discussed. The product P(AM/DMDAAC) was characterized by IR spectra、elementary analysis、TGA.
For AM/DA copolymer system,AIBA was used as initiator;Span-80/OP-10 was used as emulsifier;Cyclohexane was choosed as oil phase.The monomer DA was neutralized by hydrochloric acid.While other reaction conditions were setted, viscosity and yield of the product P(AM/ DA) were determined by Ubbelohde viscosity meter in different temperature;By parity of reasoning,viscosity and yield of the product P(AM/DA) were determined in different initiator concentration、monomer concentration and monomer ratio.Thereout the best reaction conditions were abtained. The product P(AM/DA) was represented by IR spectrum、elementary analysis、TGA、~1H-NMR and static laser light scattering.The above representation proved that AM and DA have copolymerised.Three P(AM/DA) solutions of different ratio of monomers were made acid-bases titration,the result was fundamentally accordant with ratio of monomers.
For AM/DMDAAC/AMPS copolymer system,AIBA、Span-80/OP-10、cyclohexane were separately used as initiator、emulsifier、oil phase. P(AM/DMDAAC/AMPS) was synthesized.Through experiment,the influence of initiator concentration、monomer concentration and monomer ratio on the product's viscosity and yield was studied.IR spectrum、elementary analysis、TGA were made for P(AM/DMDAAC/AMPS).The result explained that AM、DMDAAC、AMPS were copolymerized.
本文以丙烯酰胺(AM)为主要原料,分别与甲基丙烯酰氧乙基三甲基氯化铵(DMC)、二甲基二烯丙基氯化铵(DMDAAC)、二烯丙基胺(DA)、2-丙烯酰胺-2-甲基丙磺酸(AMPS)等单体进行反相乳液聚合,分别合成了AM/DMC共聚物、AM/DMDAAC共聚物、AM/DA共聚物、AM/AMPS/DMDAAC三元共聚物,并对四种不同结构特征的阳离子聚合物进行表征及性质测定。
(1)对于AM/DMC共聚物体系,采用过硫酸钾-四甲基乙二胺(KPS-TMEDA)为引发剂,Span系列乳化剂山梨糖醇酐油酸酯(Span-80)与OP系列乳化剂辛烷基酚聚氯乙烯醚(OP-10)复配作为复合乳化体系,选择环己烷为油相,合成了季铵型的P(AM/DMC)共聚物。通过实验,对反应条件进行了深入研究,确定了最佳反应温度、油水比、引发剂用量、乳化剂用量、单体浓度、单体配比,并对合成的共聚物进行了表征。将P(AM/DMC)共聚物的红外光谱与PAM的红外光谱进行了比较,发现了P(AM/DMC)共聚物的特征吸收峰;用元素分析对P(AM/DMC)共聚物的组成进行了测定;将不同单体配比的P(AM/DMC)共聚物进行了热失重分析;对P(AM/DMC)共聚物进行了核磁共振氢谱表征,谱图中的吸收峰与共聚物分子式基本吻合。以上表征说明了AM与DMC发生了很好的共聚。
(2)对于AM/DMDAAC共聚物体系,采用2-2'-偶氮(2-甲基丙基脒)二盐酸盐(AIBA)为引发剂,Span-80/OP-10为复合乳化剂,选择环己烷为油相,合成了季铵型P(AM/DMDAAC)共聚物。讨论了反应温度、引发剂浓度、单体浓度、单体配比对产物特性黏度和产率的影响。利用红外光谱、元素分析、热失重等检测手段对合成的共聚物P(AM/DMDAAC)进行了表征,结果证明加入的单体进行了很好的共聚。
(3)对于AM/DA共聚物体系,以AIBA为引发剂,Span-80/OP-10为复合乳化剂,环己烷为油相,制备了仲胺型的P(AM/DA)阳离子聚合物。反应前用盐酸中和单体DA,以防止其发生链转移。固定其它反应条件不变,用乌氏粘度计测定了在不同引发剂浓度下产物P(AM/DA)的特性黏度及产率;以此类推,测定了在不同单体浓度、单体配比条件下产物P(AM/DA)的特性黏度及产率。由此得出了制备P(AM/DA)共聚物的最佳反应条件。对产物P(AM/DA)做了红外光谱、元素分析、热失重、核磁共振氢谱、静态激光光散射表征,结果证明AM与DA发生了很好的共聚。对三种不同单体配比的共聚物溶液进行了酸碱滴定,滴定结果与元素分析结果基本吻合。
(4)对于AM/AMPS/DMDAAC共聚物体系,采用引发剂AIBA,复合乳化剂Span-80/OP-10,选择环己烷为油相,合成了两性结构的P(AM/AMPS/DMDAAC)三元共聚物。通过实验,研究了引发剂用量、单体浓度、单体配比对产物特性黏度和产率的影响。对产物P(AM/AMPS/DMDAAC)进行了红外光谱、元素分析、热失重表征,结果说明了AM与AMPS及DMDAAC发生了很好的共聚。
The inverse emulsion polymerization has the merit of high polymerization velocity、high product solidity、high molecular weight、moderate reaction conditions and so on.The inverse emulsion polymerization has widely application in adhesive、thickening agent in textile industry、flocculating agent、thickening agent、intensifier in petroleum and paper making、dope、medicine and so on.
In this paper,four kinds of cationic copolymer were synthesized by the inverse emulsion polymerization using monomers such as acrylamide(AM), methacryloxyethyl trimethyl ammonium chloride(DMC),diallyldimethylammonium chloride(DMDAAC),diallylamine(DA),2-Acrylamido-2-Methylpropane Sulfonic Acid(AMPS).The experimental conditions were studied detailedly to obtain optimum reaction conditions,including of temperature,the content of initiators ratio and content of different monomers,the content of emulsifier.
For AM/DMC copolymer system,potassium persulfate tetramethylethylenediamine(KPS-TMEDA) was used as initiator;Emulsifier sorbitan monooleate(Span-80)/Polyoxyethylene octylphenol ether(OP-10) was used as compound emulsifier;Cyclohexane was choosed as oil phase.Through experiment, the reaction conditions were studied and the best temperature、oil-water ratio、initiator concentration、emulsifier concentration、monomer concentration and monomer ratio were determined.The IR spectra of poly(AM-co-DMC) and PAM were compared, the characteristic peak of poly(AM-co-DMC) was discovered.The composition of poly(AM-co-DMC)was obtained by Elementary analysis.The copolymers poly(AM-co-DMC) of different monomer ratio were made TG analysis;Nuclear magnetic resonance of Poly(AM-co-DMC) showed that the absorption peaks were fundamentally accordant with its structure.The above representation described that AM and DMC have copolymerised.
For AM/DMDAAC copolymer system,2,2' -Azobis(2-methylpropionamide) dihydrochloride(AIBA) was used as initiator,Span80/OP-10 was used as emulsifier, Cyclohexane was choosed as oil phase.The copolymer P(AM/DMDAAC) was synthesized.The influence of temperature、initiator concentration、monomer concentration and monomer ratio on the product's viscosity and yield was discussed. The product P(AM/DMDAAC) was characterized by IR spectra、elementary analysis、TGA.
For AM/DA copolymer system,AIBA was used as initiator;Span-80/OP-10 was used as emulsifier;Cyclohexane was choosed as oil phase.The monomer DA was neutralized by hydrochloric acid.While other reaction conditions were setted, viscosity and yield of the product P(AM/ DA) were determined by Ubbelohde viscosity meter in different temperature;By parity of reasoning,viscosity and yield of the product P(AM/DA) were determined in different initiator concentration、monomer concentration and monomer ratio.Thereout the best reaction conditions were abtained. The product P(AM/DA) was represented by IR spectrum、elementary analysis、TGA、~1H-NMR and static laser light scattering.The above representation proved that AM and DA have copolymerised.Three P(AM/DA) solutions of different ratio of monomers were made acid-bases titration,the result was fundamentally accordant with ratio of monomers.
For AM/DMDAAC/AMPS copolymer system,AIBA、Span-80/OP-10、cyclohexane were separately used as initiator、emulsifier、oil phase. P(AM/DMDAAC/AMPS) was synthesized.Through experiment,the influence of initiator concentration、monomer concentration and monomer ratio on the product's viscosity and yield was studied.IR spectrum、elementary analysis、TGA were made for P(AM/DMDAAC/AMPS).The result explained that AM、DMDAAC、AMPS were copolymerized.
引文
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