水分散法制备3D打印用PP粉末的可行性
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摘要
采用水分散法制备选择性激光烧结用聚丙烯(PP)粉末,使用普朗尼克(F108)作为表面活性剂,成功验证了水分散法的可行性。对PP在水中分散效果的若干因素进行了研究,包括表面活性剂的添加量、PP的添加量、成核剂的添加量、PP的熔体流动速率等原料配比因素以及温度、搅拌转速等反应条件的影响。表面活性剂添加量少于10 g则无法得到PP粉末,在表面活性剂添加量为10~60 g范围内,表面活性剂添加量与PP成粉率成正比,表面活性剂添加量为60 g以上时,PP的成粉率变化不大;PP的添加量达到10 g以上时,PP的成粉质量在7 g左右;白炭黑作为成核剂对PP的分散效果影响很大,并且PP的成粉率在白炭黑添加量为0.15 g时达到最大值,为57.6%;PP的熔体流动速率(MFR)与其成粉率成正比,PP的MFR由20 g/(10 min)增加到41.3 g/(10 min)时,PP的成粉率由48.6%增加到56.4%。改变加热温度、降温方式对PP成粉率的影响不大,而搅拌转速对PP分散效果的影响显著,搅拌转速与PP的成粉率成正比,在搅拌转速为1 500 r/min时,PP的成粉率达到最大值,为72.5%。水分散法制备的PP粉末球形度高、表面光滑、流动性好。
Water dispersion method was used to prepare polypropylene(PP) powder for selective laser sintering,the use of Pluronic(F108) as a surfactant successfully verifies the feasibility of the water dispersion method. Several factors affecting the dispersion of PP in water were studied,the factors involve in the amount of raw materials include the amount of surfactant added,the amount of PP added,the amount of nucleating agent added,the melt flow rate(MFR) of PP and the reaction conditions including temperature,rotating speed. When the amount of surfactant is less than 10 g,the PP powder can not be obtained,and in the range of 10-60 g,it is directly proportional to the rate of PP powder formation. When the amount of surfactant is 60 g or more,the rate of PP powder formation changes little. When the amount of PP is more than 10 g,the quality of the PP powder is about 7 g. The effect of carbon-white as nucleating agent on dispersion is great,and the rate of PP powdering is the largest when the amount of carbonwhite added is 0.15 g. The MFR of PP is proportional to the pulverized rate of PP. When the MFR of PP is increased from 20 g/(10 min) to 41.3 g/(10 min),the rate of pulverization of PP is from 48.6% to 56.4%. Changing the heating temperature and the cooling method has little effect on the rate of PP powder,and the stirring speed has a significant effect on the PP dispersion effect. The speed is proportional to the rate of PP powder formation,and the maximum rate of powder formation is 72.5% at the speed of 1 500 r/min. PP powder prepared by water dispersion method has high sphericity,smooth surface and good fluidity.
Water dispersion method was used to prepare polypropylene(PP) powder for selective laser sintering,the use of Pluronic(F108) as a surfactant successfully verifies the feasibility of the water dispersion method. Several factors affecting the dispersion of PP in water were studied,the factors involve in the amount of raw materials include the amount of surfactant added,the amount of PP added,the amount of nucleating agent added,the melt flow rate(MFR) of PP and the reaction conditions including temperature,rotating speed. When the amount of surfactant is less than 10 g,the PP powder can not be obtained,and in the range of 10-60 g,it is directly proportional to the rate of PP powder formation. When the amount of surfactant is 60 g or more,the rate of PP powder formation changes little. When the amount of PP is more than 10 g,the quality of the PP powder is about 7 g. The effect of carbon-white as nucleating agent on dispersion is great,and the rate of PP powdering is the largest when the amount of carbonwhite added is 0.15 g. The MFR of PP is proportional to the pulverized rate of PP. When the MFR of PP is increased from 20 g/(10 min) to 41.3 g/(10 min),the rate of pulverization of PP is from 48.6% to 56.4%. Changing the heating temperature and the cooling method has little effect on the rate of PP powder,and the stirring speed has a significant effect on the PP dispersion effect. The speed is proportional to the rate of PP powder formation,and the maximum rate of powder formation is 72.5% at the speed of 1 500 r/min. PP powder prepared by water dispersion method has high sphericity,smooth surface and good fluidity.
引文
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[2]闫春泽,史玉升,杨劲松,等.高分子材料在选择性激光烧结中的应用——(Ⅱ)材料特性对成形的影响[J].高分子材料科学与工程,2010,26(8):145–149.Yan Chunze,Shi Yusheng,Yang Jinsong,et al.Application of Polymeric materials in selective laser sintering——(Ⅱ)Effects of polymer characteristics on forming[J].Polymeric Materials Science and Engineering,2010,26(8):145–149.
[3]史玉升,闫春泽,魏青松,等.选择性激光烧结3D打印用高分子复合材料[J].中国科学:信息科学,2015,45(2):204–211.Shi Yusheng,Yan Chunze,Wei Qingsong,et al.Polymer based composites for selective laser sintering 3D printing technology[J].Scientia Sinica Informationis,2015,45(2):204–211.
[4]李正仁.热塑性粉末涂料的生产方法[J].现代涂料与涂装,2007,10(6):38–41.Li Zhengren.Manufacture of thermoplastic powder coatings[J].Modern Paint and Finishing,2007,10(6):38–41.
[5]铁生年,李星,李昀珺.超细粉体材料的制备技术及应用[J].中国粉体技术,2009,15(3):68–72.Tie Shengnian,Li Xing,Li Yunjun.Preparation technology and application of ultrafine powder materials[J].China Powder Science and Technology,2009,15(3):68–72.
[6]龚俊,贾如磊,侯运丰.常温下低密聚乙烯的湍流超细粉碎研究[J].兰州理工大学学报,2006,32(6):79–81.Gong Jun,Jia Rulei,Hou Yunfeng.Ultra-fine comminution of LDPE with turbulence milling at atmospheric temperature[J].Journal of Lanzhou University of Technology,2006,32(6):79–81.
[7]广东银禧科技股份有限公司.选择性激光烧结聚丙烯粉末材料的制备及应用方法:中国,104031319A[P].2014-09-10.Guangdong Silver Age Sci.&Tech.Co.,Ltd..Preparation and application of selective laser sintered polypropylene powder material:CN,104031319A[P].2014-09-10.
[8]马云鹏.选择性激光烧结用聚丙烯粉末的制备研究[D].广州:广东工业大学,2016.Ma Yunpeng.Study on preparation and application in selective laser sintering of polypropylene powders[D].Guangzhou:Guangdong University of Technology,2016.
[9]汪艳.一种用于选择性激光烧结的聚丙烯粉末材料及其制备方法:中国,105802012A[P].2016-04-18.Wang Yan.Polypropylene powder material for selective laser sintering and its preparation method:CN,105802012A[P].2016-04-18.
[10]张建斌,张全福,徐春艳,等.溶剂法制备尼龙1212粉末工艺研究[J].工程塑料应用,2004,32(1):22–24.Zhang Jianbin,Zhang Quanfu,Xu Chunyan,et al.Technological research of nylon 1212 powder with solvent method[J].Engineering Plastics Application,2004,32(1):22–24.
[11]张永攀.SLS用Tg可控的PS球形颗粒的制备研究[D].广州:广东工业大学,2015.Zhang Yongpan.A study on the preparation of polystyrene microspheres with controllable glass transition temperature for selective laser sintering[D].Guangzhou:Guangdong University of Technology,2015.
[12]齐迪.用于选择性激光烧结高分子材料的制备与成型研究[D].青岛:青岛科技大学,2016.Qi Di.Study on preparation and molding of polymer materials used for selective laser sintering[D].Qingdao University of Science&Technology,2016.
[13]Schmidt J,Sachs M,Blümel C,et al.A novel process route for the production of spherical LBM polymer powders with small size and good flowability[J].Powder Technology,2014,261(261):78–86.
[14]郭宝华,陈曦,徐军,等.一种平均粒径可控的制备高堆积密度聚酰胺粉体的方法:中国,200410088820.7[P].2005-06-08.Guo Baohua,Chen Xi,Xu Jun,et al.A method for preparing high bulk density polyamide powder with controlled average particle size:CN,200410088820.7[P].2005-06-08.
[15]Mcclain D M.Process for the preparation of finely divided thermoplastic resin:US,4329304[P].1982-05-11.