CN100439423C - 低休止角粉末状乙烯基吡咯烷酮聚合物及其制造方法 - Google Patents
低休止角粉末状乙烯基吡咯烷酮聚合物及其制造方法 Download PDFInfo
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Abstract
本发明提供粉体流动性好的粉末状乙烯基吡咯烷酮聚合物及其制造方法。本发明的粉末状乙烯基吡咯烷酮聚合物为休止角小于30度的聚合物。为获得低休止角粉末状乙烯基吡咯烷酮聚合物，在干燥塔内喷雾干燥乙烯基吡咯烷酮聚合物溶液制造粉末状乙烯基吡咯烷酮聚合物，通过朝干燥塔内壁连续地或间断地送风，防止乙烯基吡咯烷酮聚合物粒子往前述干燥塔内壁上粘附。
Description
技术领域
本发明涉及粉末状乙烯基吡咯烷酮聚合物及其制造方法。
背景技术
以前，干燥乙烯基吡咯烷酮聚合物溶液制造粉末状乙烯基吡咯烷酮聚合物时使用喷雾干燥机或鼓式干燥机(参照专利文献1)。然而，使用这些方法在以往技术的条件下制得的粉末状乙烯基吡咯烷酮聚合物是松比重低、粉末流动性差的聚合物。
为了解决该问题，提出了使用圆盘式喷雾器制造粉末状乙烯基吡咯烷酮聚合物的方法(参照专利文献2)。然而，该方法虽然可以获得使粉末的松比重高的效果，但有关粉末流动性的改善仍不能得到充分的效果。
[专利文献1]特开平8-208741号公报
[专利文献2]特开2004-211033号公报
发明内容
本发明是鉴于上述背景技术而完成的，其目的在于提供粉体流动性进一步提高的粉末状乙烯基吡咯烷酮聚合物及其制造方法。
本发明的粉末状乙烯基吡咯烷酮聚合物为体止角小于30度的聚合物。
本发明的粉末状乙烯基吡咯烷酮聚合物的制造方法，是在干燥塔内喷雾干燥乙烯基吡咯烷酮聚合物溶液制造粉末状乙烯基吡咯烷酮聚合物的方法，通过朝干燥塔内壁连续地或断断续续地进行送风，防止乙烯基吡咯烷酮聚合物粒子往前述干燥塔内壁上粘附。
上述制造方法中，朝前述干燥塔内壁的送风方向与内壁的圆周方向的角度优选是5～175度以上。
本发明的低休止角粉末状乙烯基吡咯烷酮聚合物的粉体流动性良好，容易操作。即，可以管道输送粉体，进料可自动化。因此可消减使用粉末状乙烯基吡咯烷酮聚合物为原料时的经费。
采用本发明的制造方法可容易地得到有所期望的低休止角的粉末状乙烯基吡咯烷酮聚合物。
附图说明
图1是说明朝干燥塔内壁的送风方向的图。
图2是表示干燥塔内的内壁送风管配置例的示意性纵剖面图。
图3是表示干燥塔内的内壁送风管旋转方向的示意性平面图。
图4是表示内壁送风管的送风孔位置的示意性纵剖面图。
符号说明
10 干燥塔
20 内壁送风管
21 送风孔
具体实施方式
本发明所谓乙烯基吡咯烷酮聚合物，是乙烯基吡咯烷酮(N-乙烯基-2-吡咯烷酮)的均聚物或者乙烯基吡咯烷酮与其他的单体的共聚物。共聚物的场合，制成含有乙烯基吡咯烷酮单元20重量％(以下，称％)以上的共聚物。
作为构成共聚物的其他的单体，例如，可举出丙烯酸，甲基丙烯酸，丙烯酸的烷基酯(丙烯酸甲酯、丙烯酸乙酯等)、甲基丙烯酸的烷基酯(甲基丙烯酸甲酯，甲基丙烯酸乙酯等)，丙烯酸的氨基烷基酯(丙烯酸二乙氨基乙酯等)，甲基丙烯酸的氨基烷基酯，丙烯酸与二醇的单酯，甲基丙烯酸与二醇的单酯(甲基丙烯酸羟乙酯等)，丙烯酸的碱金属盐，甲基丙烯酸的碱金属盐，丙烯酸的铵盐，甲基丙烯酸的铵盐，丙烯酸的氨基烷基酯的季铵衍生物，甲基丙烯酸的氨基烷基酯的季铵衍生物，丙烯酸二乙氨基乙酯与硫酸甲酯的季铵化合物，乙烯基甲基醚，乙烯基乙基醚，乙烯基磺酸的碱金属盐，乙烯基磺酸的铵盐，苯乙烯磺酸，苯乙烯磺酸盐，烯丙基磺酸，烯丙基磺酸盐，甲基烯丙基磺酸，甲基烯丙基磺酸盐，醋酸乙烯酯，硬脂酸乙烯酯、N-乙烯基咪唑、N-乙烯基乙酰胺，N-乙烯基甲酰胺、N-乙烯基己内酰胺、N-乙烯基咔唑、丙烯酰胺、甲基丙烯酰胺、N-烷基丙烯酰胺，N-羟甲基丙烯酰胺、N，N-亚甲基双丙烯酰胺、乙二醇二丙烯酸酯、乙二醇二甲基丙烯酸酯、二乙烯基苯、乙二醇二烯丙基醚等。
本发明的低休止角粉末状乙烯基吡咯烷酮聚合物，如上述，休止角小于30度。这里所谓休止角，是粉体的一种常数，是指使粉体轻轻地落到水平面上时产生的圆锥体的母线与水平面形成的角度(粉体可形成的斜面的最大倾斜角)。通过使休止角小于30度，粉体流动性良好。为了进一步提高粉体流动性，优选体止角是25度以下。
用本发明的制造方法在喷雾干燥乙烯基吡咯烷酮聚合物溶液制造粉末状乙烯基吡咯烷酮聚合物时，通过朝干燥塔内壁连续地或间断地送风，可防止制得的球形粒子粘附在干燥塔内壁上发生变形，可获得休止角低的粉末产品。
图2、3表示本发明的制造方法使用的装置的一例的简略图。这些图中，符号10表示干燥塔。符号20表示沿干燥塔10的内壁设的内壁送风管。如图2所示，本例的干燥塔上部是圆柱形，下部是圆锥形，但干燥塔的形状不限于此。干燥塔10通常在下部设产品接受器(没图示)。在干燥塔10的内部，从上部导入风，从下部排出风。乙烯基吡咯烷酮聚合物水溶液，如白色箭头所示，向干燥塔内喷雾，边降落边干燥，在产品接受器中被回收。
内壁送风管20如图3中箭头所示，沿干燥塔10的内壁旋转。如图4所示，内壁送风管20，优选在与干燥塔10的内壁相对方向的面上设许多的送风孔21，从这些的送风孔21照箭头表示的样子喷出风。
朝干燥塔内壁的送风方向，与内壁的圆周方向相比，接近垂直方向的送风可更显著地获得本发明期望的效果。即，与图1所示的圆周方向的角度α优选是5～175℃，更优选是10～170度，特别优选约90度，即朝内壁大致垂直地吹风。
朝干燥塔内壁送风的风量，优选干燥所使用的总风量的0.001～40体积％，更优选0.005～30体积％，再优选0.01～10体积％。该风量太小或太大时，效果降低。
此外，干燥所使用的总风量没有特殊限定，但通常，每1m3干燥塔内的体积，是2～600Nm3/hr，优选是10～150Nm3/hr。
另外，朝干燥塔内壁送风的温度通常是0～300℃的范围内，优选50℃～250℃，更优选是100℃～200℃。温度低时，干燥效率差，温度太高时，存在难以得到低休止角粉末的倾向。
作为风，可适当地使用空气或惰性气体。作为产生热风的装置，有电热器、利用液化石油气等可燃性气体的燃烧热或利用重油等可燃性油的燃烧热的装置，其中，电热器或利用可燃性气体的燃烧热的场合，烟灰等造成的污染少而优选。
送风的干燥塔内壁部分的面积优选是内壁总面积的50％以上，更优选80％以上，再优选是90％以上。另外送风的部分在干燥塔上部比下部效果更好。这是因为干燥塔内壁上部的温度高的缘故。送风可以是连续地，也可以是间断地。间断地送风的场合，每1分钟送0.5次以上，送风效果好。
喷雾方法没有特殊限定。可以是圆盘式喷雾器式，也可以是喷嘴式，喷嘴式时，可使用一流体、二流体的任何一种。
以下，对本发明的实施例进行说明，但本发明不受实施例限制。
实施例1～5与比较例1
把1吨的乙烯基吡咯烷酮聚合物水溶液(ピッツコ一ルK-30L，第一工业制药(株)制，K值30，30％水溶液)导入到圆盘式喷雾器(叶轮型(VN型)、直径15.5cm，圆盘周速4900m/分)，按干燥塔的高度10m、干燥塔的塔体直径6m、热风入塔温度200℃、热风出塔温度105℃、乙烯基吡咯烷酮聚合物水溶液供给速度400L/分，并且在表1表示的条件下进行喷雾干燥。采用以下的方法评价制得的粉末状乙烯基吡略烷酮聚合物的休止角和轻打前后的松比重的比(粉体流动性)。把结果一起示于表1。再者朝干燥塔内壁的送风方向(角度α)如图1所示。
(评价方法)
休止角：使用粉末状乙烯基吡咯烷酮聚合物250ml，在25℃、湿度50％下，使用三轮式圆筒旋转法休止角测定器(筒井理化学器械(株)制)，使粉末状乙烯基吡咯烷酮聚合物与户外空气接触后，在10分钟以内进行测定。由测定值按以下的基准评价休止角。
○：小于30度
×：30度以上。
轻打前后的松比重的比：把100ml粉末状乙烯基吡咯烷酮聚合物投入到100ml量筒中，反复轻打直到体积不变化，在体积不变化的时刻测定体积。算出轻打后的体积与轻打前的体积的比(x：轻打后的体积/100)。
表1
本发明的低休止角粉末状乙烯基吡咯烷酮聚合物，适合作为各种粘合剂，整发剂，油墨，衣料用洗涤剂，治疗药等的原料使用。本聚合物由于粉体流动性好，故具有工业上作为原料进料时操作容易的优点。
Claims (1)
1.粉末状乙烯基吡咯烷酮聚合物的制造方法，其是在干燥塔内喷雾干燥乙烯基吡咯烷酮聚合物溶液而制造粉末状乙烯基吡咯烷酮聚合物的方法，其特征在于，通过朝干燥塔内壁连续地或间断地送风，防止乙烯基吡咯烷酮聚合物粒子向前述干燥塔内壁上粘附，朝前述干燥塔内壁的送风方向与内壁的圆周方向的角度是5～175度。
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| CN1517370A (zh) * | 2003-01-08 | 2004-08-04 | ��һ��ҵ��ҩ��ʽ���� | 粉末状乙烯基吡咯烷酮聚合物的制备方法 |
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| JPH11292978A (ja) * | 1998-04-06 | 1999-10-26 | Dainippon Ink & Chem Inc | 樹脂粉末の製造方法および樹脂粉末 |
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