3 lines
5.4 KiB
JSON
3 lines
5.4 KiB
JSON
{
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"protocol": "(1)称取质量比为2:1∼9:1的甲基丙烯酸二甲氨基乙酯和1,3-丙磺酸内酯，向甲基丙烯酸二甲氨基乙酯中加入1,3-丙磺酸内酯，在10∼60°C反应0.5∼4h，经过滤、抽提、干燥制得甲基丙烯酰氧乙基-N, N^-二甲基丙磺酸盐；(2)称取摩尔比为1:1.1∼1:1.3的4-乙烯基吡啶和1,3-丙磺酸内酯，准备有机溶剂和助剂，反应中有机溶剂与4-乙烯基吡啶和1,3-丙磺酸内酯的总质量比为2:1∼8:1，加入助剂后将溶剂分成三份与上述物质混合，得到的三种混合溶液依次加入反应器，在20∼90°C下反应1∼10h，经过滤、洗涤、干燥制得4-乙烯基吡啶丙磺酸内盐；(3)将步骤(1)的甲基丙烯酰氧乙基-N, N^-二甲基丙磺酸盐、丙烯酰胺和步骤(2)的4-乙烯基吡啶丙磺酸盐，按照1.5∼3:6∼7:0.5∼1.5的摩尔比加入溶剂溶解后通入N2除氧0.5∼1h，并升温至50∼70°C，恒温5∼10min后加入引发剂反应4∼6h，得到凝胶状固体，用丙酮沉淀得白色沉淀物；(4)将步骤(3)得到的沉淀物在100∼120°C下干燥16∼24h后粉碎，最终得两性离子共聚物。The text excerpt does not provide any experimental protocol for the synthesis of hydrophilic polymers with functional groups.杨小华采用MAOPS,AM和AA合成两性离子磺酸盐聚合物CPS-2000。杨金荣以氧化还原体系为引发剂,采用水溶液聚合合成了两性离子四元共聚物：聚丙烯酰胺-二甲基二烯丙基氯化铵-2-丙烯酰胺基-2-甲基丙磺酸钠-甲基丙烯酸(PADAM)，郑海洪以丙烯酰胺(AM)、2-丙烯酰胺-2-甲基丙磺酸(AMPS)、二甲基二烯丙基氯化铵(DMDAAC)和顺丁烯二酸酐(MA）为单体，采用水溶液聚合方法，以过硫酸铵/亚硫酸氢钠为引发剂合成了两性离子聚合物降滤失剂PA-1。杨文以二甲基二烯丙基氯化铵(DMDAAC)、2-丙烯酰胺基-2-甲基丙磺酸(AMPS)、马来酐(MA)、丙烯酰胺(AM）为单体，氧化还原体系为引发剂，利用水溶液聚合法合成了两性离子聚合物降滤失剂PMADA。贺爱民采用水溶液聚合方法合成的AEDMAC/AM/AA两性共聚物降滤失剂。中国专利CN2008100472416以丙烯酰胺2-丙烯酰胺基-2-甲基丙磺酸为单体，采用水溶液聚合合成了一种两性离子聚合物降滤失剂。(1)称取质量比为 2:1∼9:1 的甲基丙烯酸二甲氨基乙酯和1,3-丙磺酸内酯，并向甲基丙烯酸二甲氨基乙酯中加入1,3-丙磺酸内酯，反应在 10∼60°C 的温度下进行 0.5∼4h，最后经过滤、抽提、干燥得到甲基丙烯酰氧乙基-N,N-二甲基丙磺酸盐; (2)按照摩尔比为 1:1.1∼1:1.3 称取4-乙烯基吡啶和1,3-丙磺酸内酯，加入有机溶剂和助剂，有机溶剂与4-乙烯基吡啶和1,3-丙磺酸内酯的质量比为2:1∼8:1，助剂与总质量的比例为 0.001∼0.01，平均分三次混合后，在20°C∼90°C反应 1∼10h，经过滤、洗涤、干燥得到4-乙烯基吡啶丙磺酸内盐; (3)按 1.5∼3:6∼7:0.5∼1.5 的摩尔比称取步骤(1)的产物、丙烯酰胺和步骤(2)得到的4-乙烯基吡啶丙磺酸盐，溶解后通入N2除氧 0.5∼1h，升温至 50∼70°C，恒温 5∼10min 后加入引发剂反应 4∼6h，得到凝胶状固体，丙酮沉淀得白色沉淀; (4)将步骤(3)得到的沉淀物在 100∼120°C 下干燥 16∼24h 后粉碎，最终得到DMAPS-AM-VPPS两性离子共聚物。1. Preparation of DMAPS: Weigh 630g of DMA and place it in a reactor. Heat in a constant temperature water bath and begin stirring. Weigh 122g of PS and directly add it to DMA. The reaction temperature is 35°C, and stir for 1.5 hours to obtain the crude product of DMAPS. Transfer the crude product to filter paper, wrap it, and place it in a Soxhlet extractor using ethanol as the solvent for extraction for 1 hour. After extraction, dry the wrapped filter paper in an oven at 40°C to obtain pure DMAPS monomer with a yield of 92.8%. \\n\\n2. Preparation of VPPS: Weigh 105g of 4-VP, 125g of PS, 500g of organic solvent (benzene), and 0.75g of diethyl hydroxylamine. Divide the benzene into three equal parts, dissolving each with 4-VP, PS, and diethyl hydroxylamine respectively. Sequentially add the three solutions into the reactor and react at 70°C for 2 hours. After that, perform vacuum filtration, wash with benzene 2-3 times, and dry at 50°C for 15 hours to obtain a pale yellow solid powder product weighing 2136g. \\n\\n3. Synthesis of DMAPS/AM/VPPS copolymer: Weigh 50g of DMAPS, 60g of AM, and 40g of VPPS; dissolve in a certain amount of deionized water and transfer to a reactor with a total monomer concentration of 35%. Bubble N2 to remove oxygen for 1 hour, heat to 60°C for 30 minutes, then add 0.9g of potassium persulfate. After 6 hours, a gel-like solid is obtained, which is precipitated with acetone to yield a white precipitate. Dry at 110°C for 24 hours, then crush to obtain the DMAPS/AM/VPPS zwitterionic copolymer. \\n\\n4. Synthesis of DMAPS/AM/VPPS copolymer with NaCl: Weigh 120g of DMAPS, 60g of AM, 34g of VPPS, and 15g of NaCl; dissolve in a certain amount of deionized water and transfer to the reactor with a total monomer concentration of 30%. Bubble N2 to remove oxygen for 1 hour, heat to 55°C for 30 minutes, then add 1.4g of sodium persulfate. After 5 hours, a gel-like solid is obtained, which is precipitated with acetone to yield a white precipitate. Dry at 110°C for 24 hours, then crush to obtain the DMAPS/AM/VPPS zwitterionic copolymer."
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