棉秆粉/PVC复合材料的制备及性能研究
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摘要
木塑复合材料是以天然植物秸秆为原料,加入一些加工助剂与PVC树脂复合而成的一种环境友好型新材料,近年来得到了较快的发展,其中以木粉与PVC制备的复合材料居多。本文是利用棉花秸秆粉末为主要原料制备复合材料,研究过程包括加工工艺、提高相容性、实际应用性等几个方面,旨在获得可应用于工业化生产的棉秆粉/PVC复合材料,为农业废弃棉花秸秆的综合利用开辟新途径。经大量实验后,得到的结论如下：
1.采用响应面正交设计优化了制片工艺条件,确定最佳工艺为：温度166℃,压力25MPa,时间127s,同时得到了关于温度(X1),压力(X2),时间(X3)的三元二次回归方程：Y=42.53+1.63X1+4X2+0.45X3-5.63X12-6.46X22-1.62X32-0.62X1X2-1.1X1X3-0.82X2X3。
2.将不同含量(20/100、30/100、40/100、50/100；棉秆粉用量相对PVC用量100份时的比例)和不同粒径(60目、100目、120目、150目)的棉秆粉作为填料分别制备复合材料,对板材进行拉伸强度、断裂伸长率、弯曲强度等相关力学性能的测试,结果表明,棉秆粉的最佳用量为40份,粒径为100目。
3.采用偶联剂处理、碱处理及共聚接枝三种不同的表面处理方法对棉秆粉改性,结果表明,三种处理方法都能从不同程度上提高棉秆粉与PVC的相容性,改善了复合材料的力学性能,其中以共聚接枝法改善效果最为明显,偶联剂次之。硅烷偶联剂的最佳用量为2%,碱溶液的最佳浓度为15%,共聚接枝反应中,引发剂浓度为0.004mol/L时,表现出高的接枝率和接枝效率。
探讨了三种不同的偶联剂(铝酸酯、钛酸酯及硅烷)的表面改性效果,并进行了弯曲强度和弯曲模量的测定,结果表明,硅烷对比其他两种偶联剂有更好的改性效果,棉秆粉与PVC的相容性明显提高。
通过扫描电镜对复合材料的断面形貌和表面形貌进行观察,证实了改性处理的良好作用,通过红外微观表征,特征峰的出现同样证实了棉秆粉已被成功改性。
4.设计了四因素三水平正交实验,对主要助剂的用量进行了探讨,结果得到,影响弯曲强度的因素主次为：硬脂酸(SA)>ACR>CaSt2>CaCO3,最终确定助剂的最佳用量为：硬脂酸0.3phr, ACR8phr, CaCO3 10phr, CaSt20.5phr。
5.制备了低发泡棉秆粉/PVC复合材料,通过对密度、力学性能、流变性能的测试与分析得到：AC:ZB-530为1：5(AC 1phr), CPE含量在6%,DOP、硬脂酸及石蜡的用量分别为2phr、0.3phr和0.4phr时,复合材料表现出优良的综合性能。
6.对棉秆粉/PVC复合材料进行了应用研究(耐候),吸水性能测试、力学性能测试、维卡软化点测试及耐热性能分析,结果表明,棉秆粉/PVC复合材料有很大实际应用价值,可以应用于工业化生产,是一条农业废弃秸秆资源综合利用的新途径。
Wood-plastic composites is an environment-friendly new materials, which is processed by natural plant stalks and PVC as raw materials with some processing aids, has been rapid development in recent years, and the wood-flour/PVC composites is the most widely used in those composites. This article is the use of cotton stalks flour as raw materials preparation of composite. The research process, including processing technology, improve compatibility and the practical application, with the purpose of get a cotton stalks-flour/PVC composites, which is a new way for the comprehensive utilization of agricultural waste cotton stalks. With the large number of experiments, the conclusion is as follows:
1. The process of production was optimized by response surface methodology (RSM) to obtain the optimum conditions. It was indicated that the optimum condition was as follows: Temperature,166℃; Pressure,25MPa; Time,127s. The regression equation describing process of production was obtained by response surface methodology:Y= 42.53+1.63X1+ 4X2+0.45X3-5.63X12-6.46X22-1.62X32-0.62X1X2-1.1X1X3-0.82X2X3.
2. Different content(20/10、30/100、40/100、50/100; cotton stalks-flour/PVC) and different particle size(60 mesh,100 mesh,120 mesh,150 mesh) as filler, which were prepared for preparation of composites, and tensile strength, elongation at break, flexural strength of composites were tested. The results show that the optimum amount of cotton stalks-flour was 40phr, and particle size was 100m.
3. Coupling agent treatment, alkali treatment and graft copolymerization of three different surface treatments were used in cotton stalks-flour; the results showed that the three processing methods can improve compatibility and mechanical properties of composites, Improvement of graft copolymer of which the most obvious effect, coupling the second. The best dosage of silane coupling agent is 2%, the best concentration of alkali solution is 15%, in the graft copolymerization reaction, the initiator concentration of 0.004mol/L, show a high grafting percentage and grafting efficiency.
Explored three different coupling agent (Al ester, titanate and silane) surface modification effect, which were used to preparation of composites, flexural strength and elastic modulus of cotton stalks-flour/PVC composites were tested. The results show that the silane coupling agent compared with the other two had the better modification effect, the compatibility of cotton stalks-flour and PVC has improved significantly.
Fracture surface and surface morphology of cotton stalks-flour/PVC composites were observed by SEM, which confirmed the positive role of modification, the emergence of characteristic peaks of cotton stalks-flour by FTIR also confirmed that has been successfully modified.
4. With orthogonal experiments, the amounts of the main additives were discussed; the results show primary and secondary factors that affect the flexural strength was as follows: SA>ACR> CaSt2> CaCO3, ultimately determine the optimum dosage of additives as:stearic acid 0.3phr, ACR 8phr, CaCO3 10phr, CaSt2 0.5phr.
5. Low foaming cotton stalks-flour/PVC composites was prepared, through testing and analysis the density, mechanical properties and rheological properties of that, It was indicated that AC:ZB-530 is 1:5 (AC lphr), CPE content of 6%, DOP, the amount of stearic acid and paraffin were 2phr,0.3phr and 0.4phr, the composite material exhibits excellent overall performance.
6. With the research on Applications of cotton stalks-flour/PVC composites (weather resistance), through water absorption test, mechanical property test, vicat softening point test and heat resistance test, the results show that the cotton stalks-flour/PVC composite have great practical value, which can be applied to industrial production and that is a new way for comprehensive utilization of resources on agricultural waste straw.
1.采用响应面正交设计优化了制片工艺条件,确定最佳工艺为：温度166℃,压力25MPa,时间127s,同时得到了关于温度(X1),压力(X2),时间(X3)的三元二次回归方程：Y=42.53+1.63X1+4X2+0.45X3-5.63X12-6.46X22-1.62X32-0.62X1X2-1.1X1X3-0.82X2X3。
2.将不同含量(20/100、30/100、40/100、50/100；棉秆粉用量相对PVC用量100份时的比例)和不同粒径(60目、100目、120目、150目)的棉秆粉作为填料分别制备复合材料,对板材进行拉伸强度、断裂伸长率、弯曲强度等相关力学性能的测试,结果表明,棉秆粉的最佳用量为40份,粒径为100目。
3.采用偶联剂处理、碱处理及共聚接枝三种不同的表面处理方法对棉秆粉改性,结果表明,三种处理方法都能从不同程度上提高棉秆粉与PVC的相容性,改善了复合材料的力学性能,其中以共聚接枝法改善效果最为明显,偶联剂次之。硅烷偶联剂的最佳用量为2%,碱溶液的最佳浓度为15%,共聚接枝反应中,引发剂浓度为0.004mol/L时,表现出高的接枝率和接枝效率。
探讨了三种不同的偶联剂(铝酸酯、钛酸酯及硅烷)的表面改性效果,并进行了弯曲强度和弯曲模量的测定,结果表明,硅烷对比其他两种偶联剂有更好的改性效果,棉秆粉与PVC的相容性明显提高。
通过扫描电镜对复合材料的断面形貌和表面形貌进行观察,证实了改性处理的良好作用,通过红外微观表征,特征峰的出现同样证实了棉秆粉已被成功改性。
4.设计了四因素三水平正交实验,对主要助剂的用量进行了探讨,结果得到,影响弯曲强度的因素主次为：硬脂酸(SA)>ACR>CaSt2>CaCO3,最终确定助剂的最佳用量为：硬脂酸0.3phr, ACR8phr, CaCO3 10phr, CaSt20.5phr。
5.制备了低发泡棉秆粉/PVC复合材料,通过对密度、力学性能、流变性能的测试与分析得到：AC:ZB-530为1：5(AC 1phr), CPE含量在6%,DOP、硬脂酸及石蜡的用量分别为2phr、0.3phr和0.4phr时,复合材料表现出优良的综合性能。
6.对棉秆粉/PVC复合材料进行了应用研究(耐候),吸水性能测试、力学性能测试、维卡软化点测试及耐热性能分析,结果表明,棉秆粉/PVC复合材料有很大实际应用价值,可以应用于工业化生产,是一条农业废弃秸秆资源综合利用的新途径。
Wood-plastic composites is an environment-friendly new materials, which is processed by natural plant stalks and PVC as raw materials with some processing aids, has been rapid development in recent years, and the wood-flour/PVC composites is the most widely used in those composites. This article is the use of cotton stalks flour as raw materials preparation of composite. The research process, including processing technology, improve compatibility and the practical application, with the purpose of get a cotton stalks-flour/PVC composites, which is a new way for the comprehensive utilization of agricultural waste cotton stalks. With the large number of experiments, the conclusion is as follows:
1. The process of production was optimized by response surface methodology (RSM) to obtain the optimum conditions. It was indicated that the optimum condition was as follows: Temperature,166℃; Pressure,25MPa; Time,127s. The regression equation describing process of production was obtained by response surface methodology:Y= 42.53+1.63X1+ 4X2+0.45X3-5.63X12-6.46X22-1.62X32-0.62X1X2-1.1X1X3-0.82X2X3.
2. Different content(20/10、30/100、40/100、50/100; cotton stalks-flour/PVC) and different particle size(60 mesh,100 mesh,120 mesh,150 mesh) as filler, which were prepared for preparation of composites, and tensile strength, elongation at break, flexural strength of composites were tested. The results show that the optimum amount of cotton stalks-flour was 40phr, and particle size was 100m.
3. Coupling agent treatment, alkali treatment and graft copolymerization of three different surface treatments were used in cotton stalks-flour; the results showed that the three processing methods can improve compatibility and mechanical properties of composites, Improvement of graft copolymer of which the most obvious effect, coupling the second. The best dosage of silane coupling agent is 2%, the best concentration of alkali solution is 15%, in the graft copolymerization reaction, the initiator concentration of 0.004mol/L, show a high grafting percentage and grafting efficiency.
Explored three different coupling agent (Al ester, titanate and silane) surface modification effect, which were used to preparation of composites, flexural strength and elastic modulus of cotton stalks-flour/PVC composites were tested. The results show that the silane coupling agent compared with the other two had the better modification effect, the compatibility of cotton stalks-flour and PVC has improved significantly.
Fracture surface and surface morphology of cotton stalks-flour/PVC composites were observed by SEM, which confirmed the positive role of modification, the emergence of characteristic peaks of cotton stalks-flour by FTIR also confirmed that has been successfully modified.
4. With orthogonal experiments, the amounts of the main additives were discussed; the results show primary and secondary factors that affect the flexural strength was as follows: SA>ACR> CaSt2> CaCO3, ultimately determine the optimum dosage of additives as:stearic acid 0.3phr, ACR 8phr, CaCO3 10phr, CaSt2 0.5phr.
5. Low foaming cotton stalks-flour/PVC composites was prepared, through testing and analysis the density, mechanical properties and rheological properties of that, It was indicated that AC:ZB-530 is 1:5 (AC lphr), CPE content of 6%, DOP, the amount of stearic acid and paraffin were 2phr,0.3phr and 0.4phr, the composite material exhibits excellent overall performance.
6. With the research on Applications of cotton stalks-flour/PVC composites (weather resistance), through water absorption test, mechanical property test, vicat softening point test and heat resistance test, the results show that the cotton stalks-flour/PVC composite have great practical value, which can be applied to industrial production and that is a new way for comprehensive utilization of resources on agricultural waste straw.
引文
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