AM-DMC共聚物的合成與表征
發(fā)布時(shí)間：2018-10-16 09:59
【摘要】：水污染是人類21世紀(jì)面臨的重大問(wèn)題之一,廢水治理是解決水污染及水資源短缺的有效途徑,研究開(kāi)發(fā)高效、多功能陽(yáng)離子絮凝劑對(duì)處理高濁廢水具有重要的理論意義和應(yīng)用價(jià)值。雙水相聚合法具有過(guò)程溫和、可控條件多、易于操作和放大生產(chǎn),在分離提純以及機(jī)理解釋中可借助傳統(tǒng)溶劑萃取理論和經(jīng)驗(yàn)等特點(diǎn)。陽(yáng)離子型聚丙烯酰胺系列是目前我國(guó)水處理劑中用量最大的試劑之一,丙烯酰胺(AM)-甲基丙烯酰氧乙基三甲基氯化銨(DMC)共聚物(P(AM-DMC))便是陽(yáng)離子型聚丙烯酰胺中的一種,具有電荷度可控,電荷分布均勻,水處理中用量小,絮凝澄清速度快,產(chǎn)生污泥量少,處理效率高,使用后易被環(huán)境中微生物所降解等特點(diǎn),被廣泛應(yīng)用于各種工業(yè)和生活廢水的處理。本文通過(guò)大量的文獻(xiàn)閱讀,在國(guó)內(nèi)外已有研究的基礎(chǔ)上,以丙烯酰胺、甲基丙烯酰氧乙基三甲基氯化銨為共聚單體,過(guò)硫酸銨-亞硫酸氫鈉氧化還原體系為自由基引發(fā)劑,雙水相共聚法制備P(AM-DMC)陽(yáng)離子聚丙烯酰胺絮凝劑。研究共聚反應(yīng)工藝條件的優(yōu)化,雙水相共聚相關(guān)理論,對(duì)共聚反應(yīng)及共聚產(chǎn)物的結(jié)構(gòu)與性能進(jìn)行表征,并將所得共聚產(chǎn)物用于模擬廢水的治理,獲得了有意義的結(jié)論。(1)采用單因素試驗(yàn)探索聚合反應(yīng)條件,并考察單體總量、引發(fā)劑用量、單體配比、pH值、反應(yīng)時(shí)間、PEG用量等因素對(duì)共聚反應(yīng)產(chǎn)物粘均分子量和陽(yáng)離子度的影響。設(shè)計(jì)4因素3水平正交實(shí)驗(yàn),探究制備較高粘均分子量和較大陽(yáng)離子度的陽(yáng)離子聚丙烯酰胺的最佳工藝條件。(2)研究了AM-DMC二元共聚反應(yīng)的共聚物組成與單體組成之間的關(guān)系(二元共聚物微分方程),按照K-T法、F-R法、FBR法計(jì)算出單體AM和DMC在共聚反應(yīng)過(guò)程中的競(jìng)聚率,研究共聚過(guò)程的聚合類型以及利用單體競(jìng)聚率繪制單體組成與共聚物組成F-f圖。(3)探究繪制了雙水相聚合體系液/液邊界圖,研究雙水相體系分相時(shí)兩高聚物質(zhì)量分?jǐn)?shù)關(guān)系,繪制分相圖,同時(shí)對(duì)AM-DMC共聚反應(yīng)動(dòng)力學(xué)進(jìn)行了研究,得出聚合反應(yīng)動(dòng)力學(xué)曲線。(4)將最終合成產(chǎn)物在模擬和實(shí)際污水處理中進(jìn)行實(shí)際應(yīng)用,研究最終合成產(chǎn)物的性能及相關(guān)特性指標(biāo)。從單因素實(shí)驗(yàn)可知,共聚產(chǎn)物陽(yáng)離子度與粘均分子量有如下結(jié)論:隨著pH值增大先增后下降,pH控制在6.0左右最為合適;隨著單體總量的增加均為增加;其中陽(yáng)離子度隨單體總量變化影響不大。隨著反應(yīng)時(shí)間增加均為增加趨勢(shì)。但反應(yīng)時(shí)間在165min時(shí),反應(yīng)接近停止,反應(yīng)時(shí)間不要超過(guò)180min為宜。隨著引發(fā)劑用量大于2.5ml時(shí),兩個(gè)指標(biāo)都有明顯的下降趨勢(shì);隨著PEG含量的增加,聚合物的粘均分子量先增加后減小,在8%存在峰值。而陽(yáng)離子度先減小后增加。由正交試驗(yàn)可知:在總單體質(zhì)量分?jǐn)?shù)為4%,質(zhì)量比m(AM):m(DMC)=3:1,pH=9,引發(fā)劑用量為1.5mL,反應(yīng)溫度為35℃的最優(yōu)條件下,合成的P(AM-DMC)的粘均分子量最大可達(dá)1.6*106,在總單體質(zhì)量分?jǐn)?shù)為8%,AM與DMC配比m(AM):m(DMC)=3:1,pH=5,引發(fā)劑用量為2.5mL,反應(yīng)溫度為35℃的最優(yōu)條件下,合成的P(AM-DMC)的陽(yáng)離子度最大可達(dá)13.8%。在最佳工藝條件下,所得的P(AM-DMC)也具有良好的絮凝效果。模擬高嶺土懸濁液、PVSK懸濁液和AgI懸濁液三種廢水的去濁實(shí)驗(yàn),濁度去濁率均能達(dá)到70%以上。通過(guò)競(jìng)聚率設(shè)計(jì)實(shí)驗(yàn)測(cè)得DMC的競(jìng)聚率r1=2.041,AM的競(jìng)聚率r2=0.315。并且繪制出共聚反應(yīng)F-f曲線圖、共聚反應(yīng)動(dòng)力學(xué)曲線圖以及PCAM-PEG雙水相相圖。
[Abstract]:Water pollution is one of the major problems facing mankind in the 21st century. Wastewater treatment is an effective way to solve water pollution and shortage of water resources. The double-water phase-gathering method has the characteristics of mild process, multiple controllable conditions, easy operation and amplification production, and can be used in separation and purification as well as mechanism interpretation with the aid of traditional solvent extraction theory and experience. The cationic polylactide series is one of the most used reagents in the water treatment agent in China, and the poly (AM)-methylpropenoate (DMC) copolymer (P (AM-DMC)) is one of the cationic polyacetal resins, and has the advantages of controllable charge degree, uniform charge distribution, in that wat treatment, the dosage is small, the flocculation clarification speed is high, the sludge amount is low, the treatment efficiency is high, the microorganism in the environment is easy to degrade after use and the like, and is widely applied to the treatment of various industrial and domestic wastewater. In this paper, a lot of literature reading, based on the existing research at home and abroad, is taken as the free radical initiator through the oxidation reduction system of poly (ethylene glycol)-sodium bisulfite as comonomer, methyl propylene and ethyl trimethylamine as comonomer. P (AM-DMC) cationic polyacrylate flocculant was prepared by double-aqueous phase copolymerization. The structure and properties of copolymerization reaction and copolymerization product were characterized by the optimization of the process conditions of copolymerization reaction and the theory of double water phase copolymerization, and the obtained copolymer was used to simulate the treatment of wastewater. (1) Single factor test was used to explore the polymerization conditions, and the effects of monomer total amount, initiator dosage, monomer ratio, pH value, reaction time, PEG dosage and other factors on the viscosity average molecular weight and cationic degree of the copolymerization product were investigated. The optimum technological conditions for preparing cationic polylactide with higher viscosity average molecular weight and higher cationic degree were studied by designing 4 factors 3 level orthogonal experiment. (2) The relationship between copolymer composition and monomer composition of AM-DMC binary copolymerization is studied (binary copolymer differential equation), and the reactivity of monomer AM and DMC in copolymerization reaction is calculated according to K-T method, F-R method and FBR method. The polymerization type of the copolymerization process and the monomer composition and the copolymer composition F-f were studied by using the monomer reactivity ratio. (3) The liquid/ liquid boundary map of the double-aqueous phase polymerization system was studied, the relationship between the mass fraction of the two polymers was studied, the phase diagram was drawn, and the kinetics of the copolymerization of AM-DMC was studied, and the kinetics curve of polymerization was obtained. (4) carrying out practical application on the final synthesis product in the simulation and the actual sewage treatment to study the performance and the related characteristic indexes of the final synthesis product. It can be seen from the single factor experiment that the cationic degree and the viscosity average molecular weight of the copolymer are as follows: with the increase of the pH value, the pH control is most appropriate at about 6.0; with the increase of the total amount of monomer, the cationic degree is not much influenced by the total amount of monomer. As the reaction time increased, the trend was increased. but when the reaction time is 165min, the reaction is close to stop, and the reaction time is not more than 180min. With the increase of PEG content, the viscosity average molecular weight of polymer decreased first, and peak value was found in 8%. and the cationic degree is increased first. The average molecular weight of the synthesized P (AM-DMC) was 1. 6 * 106, the mass fraction of the total monomer was 8%, and the ratio of AM to DMC (AM): m (DMC) = 3: 1. The cationic degree of the synthesized P (AM-DMC) can reach 13. 8% under the optimal conditions of pH = 5, initiator dosage of 2.5mL and reaction temperature of 35 鈩，
本文編號(hào)：2274000
[Abstract]:Water pollution is one of the major problems facing mankind in the 21st century. Wastewater treatment is an effective way to solve water pollution and shortage of water resources. The double-water phase-gathering method has the characteristics of mild process, multiple controllable conditions, easy operation and amplification production, and can be used in separation and purification as well as mechanism interpretation with the aid of traditional solvent extraction theory and experience. The cationic polylactide series is one of the most used reagents in the water treatment agent in China, and the poly (AM)-methylpropenoate (DMC) copolymer (P (AM-DMC)) is one of the cationic polyacetal resins, and has the advantages of controllable charge degree, uniform charge distribution, in that wat treatment, the dosage is small, the flocculation clarification speed is high, the sludge amount is low, the treatment efficiency is high, the microorganism in the environment is easy to degrade after use and the like, and is widely applied to the treatment of various industrial and domestic wastewater. In this paper, a lot of literature reading, based on the existing research at home and abroad, is taken as the free radical initiator through the oxidation reduction system of poly (ethylene glycol)-sodium bisulfite as comonomer, methyl propylene and ethyl trimethylamine as comonomer. P (AM-DMC) cationic polyacrylate flocculant was prepared by double-aqueous phase copolymerization. The structure and properties of copolymerization reaction and copolymerization product were characterized by the optimization of the process conditions of copolymerization reaction and the theory of double water phase copolymerization, and the obtained copolymer was used to simulate the treatment of wastewater. (1) Single factor test was used to explore the polymerization conditions, and the effects of monomer total amount, initiator dosage, monomer ratio, pH value, reaction time, PEG dosage and other factors on the viscosity average molecular weight and cationic degree of the copolymerization product were investigated. The optimum technological conditions for preparing cationic polylactide with higher viscosity average molecular weight and higher cationic degree were studied by designing 4 factors 3 level orthogonal experiment. (2) The relationship between copolymer composition and monomer composition of AM-DMC binary copolymerization is studied (binary copolymer differential equation), and the reactivity of monomer AM and DMC in copolymerization reaction is calculated according to K-T method, F-R method and FBR method. The polymerization type of the copolymerization process and the monomer composition and the copolymer composition F-f were studied by using the monomer reactivity ratio. (3) The liquid/ liquid boundary map of the double-aqueous phase polymerization system was studied, the relationship between the mass fraction of the two polymers was studied, the phase diagram was drawn, and the kinetics of the copolymerization of AM-DMC was studied, and the kinetics curve of polymerization was obtained. (4) carrying out practical application on the final synthesis product in the simulation and the actual sewage treatment to study the performance and the related characteristic indexes of the final synthesis product. It can be seen from the single factor experiment that the cationic degree and the viscosity average molecular weight of the copolymer are as follows: with the increase of the pH value, the pH control is most appropriate at about 6.0; with the increase of the total amount of monomer, the cationic degree is not much influenced by the total amount of monomer. As the reaction time increased, the trend was increased. but when the reaction time is 165min, the reaction is close to stop, and the reaction time is not more than 180min. With the increase of PEG content, the viscosity average molecular weight of polymer decreased first, and peak value was found in 8%. and the cationic degree is increased first. The average molecular weight of the synthesized P (AM-DMC) was 1. 6 * 106, the mass fraction of the total monomer was 8%, and the ratio of AM to DMC (AM): m (DMC) = 3: 1. The cationic degree of the synthesized P (AM-DMC) can reach 13. 8% under the optimal conditions of pH = 5, initiator dosage of 2.5mL and reaction temperature of 35 鈩，
本文編號(hào)：2274000
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