羧甲基纤维素接枝共聚物的制备及性能研究
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摘要
羧甲基纤维素是一类能够生物降解、无毒性、抗盐性强、可再生且便宜易得的产物。对羧甲基纤维素进行接枝共聚改性，可以赋予其某些新的性能，同时又不会破坏羧甲基纤维素材料所固有的优点。本文分别考察了以羧甲基纤维素和单体丙烯酰胺为主体的CMC-AM接枝聚合反应，研究了接枝聚合反应条件和引发体系，并对其它单体与羧甲基纤维素的接枝聚合反应进行了探讨。通过红外分析、热分析、X-衍射分析等方法，充分验证了聚合物的结构，并对接枝聚合物的性质也进行了研究。
AM为主，CMC为辅的接枝聚合反应，以(NH_4)_2S_2O8-NA_2SO_3作为引发体系，研究了接枝聚合反应的条件，得出了最佳实验条件为：反应物浓度=20％、引发剂浓度=300mg/L、初始温度=40℃、初始pH值=8。各因素对聚合物分子量、接枝率的影响大小为：初始pH值＞引发剂用量＞反应物浓度＞初始温度。实验证明：在CMC比率为10％和最佳实验条件下，进行接枝聚合反应，接枝聚合物分子量达到最大值8.04×10~6，接枝率也达到了最大值845.6％，与理论值900％接近，接枝效果较好。
CMC为主，单体为辅的接枝聚合反应，对引发体系进行了研究，得出了最佳引发体系：H_2SO_4-KMnO_4，最佳引发体系的最佳引发浓度：[H_2SO_4]0.02mol/L、[KMnO_4]3.0×10~(-3)mol/L。并得到了单体浓度在7％以下，H_2SO_4-KMnO_4引发的效果较好，单体浓度在7％以上，(NH_4)_2S_2O_8-Na_2SO_3的引发效果较好的结论。同时还采用(NH_4)_2S_2O_8-Na_2SO_3([(NH_4)_2S_2O_8]300mg/L、[Na_2SO_3]300mg/L)和H_2SO_4-KMnO_4([H_2SO_4]0.02mol/L、[KMnO_4]3.0×10~(-3)mol/L)混合引发的方式对接枝聚合物进行引发，实验表明：混合引发较其中(NH_4)_2S_2O_8-Na_2SO_3单独引发的效果有明显增强。
对其它单体与丙烯酰胺的接枝聚合反应进行研究表明，醋酸乙烯酯、乙二胺作为羧甲基纤维素接枝单体不合适。对于烯丙基类单体，实验证明其接枝能力：丙烯酰胺＞丙烯酸钠＞丙烯酸甲酯。
对接枝共聚物进行了性能测定，证明了接枝聚合物的抗盐性、耐温性较单纯的CMC和PAM有了显著提高。并且通过特性粘数、回旋半径、电导的测试，得出了接枝聚合物的最佳组成：CMC比率15％，水解度15％。
CMC is a product of biological degradation , no-toxicity, salt-resistance, regeneration and inexpensive. As for the modification of CMC graft copolymerization, we can endow it with some new properties while virtues which CMC inhered with can't be destroyed. This paper studies the reaction of CMC-AM graft copolymerization which has taken the main reactive part as CMC or AM respectively, the conditions of graft copolymerization and initiation systems, and some monomers grafted onto CMC. It is fully approved the construction of polymers by means of the FT-IR analysis, thermal analysis, X-ray diffraction analysis and so on. This paper also researches the properties of graft copolymers.
The reaction of graft copolymerization initiated by (NH4)2S2O8-Na2SO3 , which has the main reactive part of AM and minor reactive part of CMC, has studied the reaction conditions. The results show that the optimal reaction conditions should be: the reaction compound concentration is 20%; the initiator concentration is 300mg/L; the initial temperature is 40℃; the initial pH value is 8. The priority of the effects is: the initial pH value, the initiator concentration, the reaction compound concentration, the initial temperature. The experiences approve that at the ratio of CMC is 10% and the optimal reaction conditions, we can get the best molecular weigh of 8.03×106 and the degree of grafting achieved the best value of 845.6% as well, which is similar with the theoretical value of 900%.So we can conclude that the effect of graft is very well.
We study the initiation systems of the graft reaction which has the main reactive part of CMC and the secondary reactive part of monomers, and get the optimal initiation system: [H2SO4] 0.02mol/L,[KMnO4] 3.0×10-3 mol/L.We also get some other conclusions: under the monomer concentration of 7%, initiation system of H2SO4-KMnO4 has the best initiation effect, but (NH4)S2O8-Na2SO3 has the best initiation effect above the monomer concentration of 7%. Meanwhile, we initiate the graft copolymerization by means of mixed initiations: (NH4)2S2O8-Na2SO3 ([(NH4)2S2O8] 300mg/L,[Na2SO3] 300mg/L)and H2SO4-KMnO4([H2SO4] 0.02mol/L.[KMnO4] 3.0×10-3 mol/L),the result shows that the effect of mixed initiations has do
better than simple initiation of H2SO4-KMnO4.
As for other monomers grafted onto CMC, vinyl acetate and ethylenediamine are not suitable to graft onto CMC, while some other allyl monomers, the priority of the effects is acrylamide, sodium acrylate, methyl acryalate.
We study the properties of graft copolymers and have verified that the salt-resistance and heat-resistance of graft copolymers have improved remarkably than CMC or PAM alone. According to the properties of viscosity, radius of gyration and conductivity, we have achieved the best components,which the ratio of CMC is 15% and the hydrolysis degree of graft copolymer is 15%.
AM为主，CMC为辅的接枝聚合反应，以(NH_4)_2S_2O8-NA_2SO_3作为引发体系，研究了接枝聚合反应的条件，得出了最佳实验条件为：反应物浓度=20％、引发剂浓度=300mg/L、初始温度=40℃、初始pH值=8。各因素对聚合物分子量、接枝率的影响大小为：初始pH值＞引发剂用量＞反应物浓度＞初始温度。实验证明：在CMC比率为10％和最佳实验条件下，进行接枝聚合反应，接枝聚合物分子量达到最大值8.04×10~6，接枝率也达到了最大值845.6％，与理论值900％接近，接枝效果较好。
CMC为主，单体为辅的接枝聚合反应，对引发体系进行了研究，得出了最佳引发体系：H_2SO_4-KMnO_4，最佳引发体系的最佳引发浓度：[H_2SO_4]0.02mol/L、[KMnO_4]3.0×10~(-3)mol/L。并得到了单体浓度在7％以下，H_2SO_4-KMnO_4引发的效果较好，单体浓度在7％以上，(NH_4)_2S_2O_8-Na_2SO_3的引发效果较好的结论。同时还采用(NH_4)_2S_2O_8-Na_2SO_3([(NH_4)_2S_2O_8]300mg/L、[Na_2SO_3]300mg/L)和H_2SO_4-KMnO_4([H_2SO_4]0.02mol/L、[KMnO_4]3.0×10~(-3)mol/L)混合引发的方式对接枝聚合物进行引发，实验表明：混合引发较其中(NH_4)_2S_2O_8-Na_2SO_3单独引发的效果有明显增强。
对其它单体与丙烯酰胺的接枝聚合反应进行研究表明，醋酸乙烯酯、乙二胺作为羧甲基纤维素接枝单体不合适。对于烯丙基类单体，实验证明其接枝能力：丙烯酰胺＞丙烯酸钠＞丙烯酸甲酯。
对接枝共聚物进行了性能测定，证明了接枝聚合物的抗盐性、耐温性较单纯的CMC和PAM有了显著提高。并且通过特性粘数、回旋半径、电导的测试，得出了接枝聚合物的最佳组成：CMC比率15％，水解度15％。
CMC is a product of biological degradation , no-toxicity, salt-resistance, regeneration and inexpensive. As for the modification of CMC graft copolymerization, we can endow it with some new properties while virtues which CMC inhered with can't be destroyed. This paper studies the reaction of CMC-AM graft copolymerization which has taken the main reactive part as CMC or AM respectively, the conditions of graft copolymerization and initiation systems, and some monomers grafted onto CMC. It is fully approved the construction of polymers by means of the FT-IR analysis, thermal analysis, X-ray diffraction analysis and so on. This paper also researches the properties of graft copolymers.
The reaction of graft copolymerization initiated by (NH4)2S2O8-Na2SO3 , which has the main reactive part of AM and minor reactive part of CMC, has studied the reaction conditions. The results show that the optimal reaction conditions should be: the reaction compound concentration is 20%; the initiator concentration is 300mg/L; the initial temperature is 40℃; the initial pH value is 8. The priority of the effects is: the initial pH value, the initiator concentration, the reaction compound concentration, the initial temperature. The experiences approve that at the ratio of CMC is 10% and the optimal reaction conditions, we can get the best molecular weigh of 8.03×106 and the degree of grafting achieved the best value of 845.6% as well, which is similar with the theoretical value of 900%.So we can conclude that the effect of graft is very well.
We study the initiation systems of the graft reaction which has the main reactive part of CMC and the secondary reactive part of monomers, and get the optimal initiation system: [H2SO4] 0.02mol/L,[KMnO4] 3.0×10-3 mol/L.We also get some other conclusions: under the monomer concentration of 7%, initiation system of H2SO4-KMnO4 has the best initiation effect, but (NH4)S2O8-Na2SO3 has the best initiation effect above the monomer concentration of 7%. Meanwhile, we initiate the graft copolymerization by means of mixed initiations: (NH4)2S2O8-Na2SO3 ([(NH4)2S2O8] 300mg/L,[Na2SO3] 300mg/L)and H2SO4-KMnO4([H2SO4] 0.02mol/L.[KMnO4] 3.0×10-3 mol/L),the result shows that the effect of mixed initiations has do
better than simple initiation of H2SO4-KMnO4.
As for other monomers grafted onto CMC, vinyl acetate and ethylenediamine are not suitable to graft onto CMC, while some other allyl monomers, the priority of the effects is acrylamide, sodium acrylate, methyl acryalate.
We study the properties of graft copolymers and have verified that the salt-resistance and heat-resistance of graft copolymers have improved remarkably than CMC or PAM alone. According to the properties of viscosity, radius of gyration and conductivity, we have achieved the best components,which the ratio of CMC is 15% and the hydrolysis degree of graft copolymer is 15%.
引文
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