CN202543125U - 一种连续法生产热塑性聚氨酯弹性体的*** - Google Patents
一种连续法生产热塑性聚氨酯弹性体的*** Download PDFInfo
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Abstract
本实用新型公开了一种连续法生产热塑性聚氨酯弹性体的***,其特点是它包括储料罐(1)、浇注机(2)、挤出机(3)、带式反应器(4)、粉碎机(5)和包装机(6),所述挤出机(3)和带式反应器(4)之间通过连接器(7)连接;所述挤出机(3)为双螺杆挤出机或单螺杆挤出机;所述带式反应器(4)为带加温功能的钢带或者聚四氟乙烯带;采用挤出机和带式反应器逐步反应合成热塑性聚氨酯弹性体,挤出机用来完成前期混合和初期反应,带式反应器提供后期反应和结晶,通过分段反应,物料停留时间能够调节,给予物料充分的结晶时间,可对TPU的分子量进行控制,有效的消除凝胶化现象,制造的TPU粒料均一,具有非常好的物理机械性能。
Description
技术领域:
本实用新型涉及高分子聚合物制备技术领域,具体地讲是一种连续法生产热塑性聚氨酯弹性体的***。
背景技术:
热塑性聚氨酯弹性体(TPU)具有良好的弹性体性能和可热塑加工性,被广泛应用于汽车部件、密封件、医疗用具、电缆、管材、消防水带、鞋材等领域。如在山西省化工研究所编著的《聚氨酯弹性体手册》(化学工业出版社,2005,P398)中详细介绍了有关TPU制备、性能与应用。
众所周知的制备工艺是双螺杆挤出机工艺,该法是将原料计量加入到双螺杆反应器中聚合并造粒。传统的双螺杆挤出机工艺存在以下问题:1、这种挤出工艺比较简单,混合和反应同时进行,但是以这种方式制得的产物均一性差;2、物料在挤出机内的停留时间有限,一般小于1分钟,使反应难于控制,导致产品反应不完全或者出现凝胶;3、起始原料在反应器中反应温度较高,容易发生不希望且不可控的交联脲基甲酸酯次级反应。
为了不断提高TPU的品质,满足多方面的需求,很多TPU生产企业都积极致力于生产工艺的改进。bayer公司在CN1281474中通过预聚体工艺来生产TPU,主要是先将多元醇和异氰酸酯在管式反应器反应生成预聚物,后期将预聚物同扩链剂在双螺杆反应器中反应生成TPU,但是后期扩链反应全部通过双螺杆高温反应,导致产生不均一以及不可控的次级反应。同时由于预聚物粘度大,影响计量,操作复杂,清理困难,导致无法得到满意的效果。
德国拜尔公司在专利CN1289561C中公布了一种热塑性聚氨酯弹性体多阶段连续制备技术。该技术主要过程如下:首先将部分多元醇同异氰酸酯由静态混合器混合生成预聚物,然后将该预聚物同剩余多元醇由静态混合器混合后经过管状反应器反应,生成物直接加入到双螺杆的入口处同扩链剂在双螺杆中进行反应,最终将全部物料挤出造粒制得成品TPU。该工艺较传统的双螺杆工艺能够制备组成更加复杂的TPU,但该方法操作工艺繁琐复杂,给实际生产控制方面提出了更高的要求。同时也无法避免后期的高温反应以及交联反应的生成。烟台万华新材料科技有限公司在专利CN101020737中试图通过双阶机延长在螺杆中的停留时间,但是由于高温反应,导致凝胶较多,产品均一性差。
目前的双螺杆工艺以及预聚体工艺均没有有效地对TPU后期反应进行控制,因此容易产生超大分子,产品不均一,容易生成不溶物和凝胶。
实用新型内容:
本实用新型的目的是克服上述已有技术的不足,而提供一种连续法生产热塑性聚氨酯弹性体的***,主要解决现有的双螺杆工艺以及预聚体工艺连续生产热塑性聚氨酯弹性体由于没有有效地对TPU后期反应进行控制,容易产生超大分子,产品不均一,容易生成不溶物和凝胶等问题。
本实用新型的技术方案是:一种连续法生产热塑性聚氨酯弹性体的***,其特殊之处在于它包括储料罐、浇注机、挤出机、带式反应器、粉碎机和包装机,所述挤出机和带式反应器之间通过连接器连接;所述挤出机为双螺杆挤出机或单螺杆挤出机,螺杆挤出机提供前期混合和初期反应;所述带式反应器为带加温功能的钢带或者聚四氟乙烯带,带式反应器提供后期反应和结晶。
进一步的,所述单螺杆和双螺杆挤出机均可用于反应挤出,因反应开始物料的混合程度对反应结果影响重大,而挤出机机段主要起着混合物料使物料初期反应的作用,因此挤出机机段最佳选择是双螺杆挤出机;双螺杆挤出机为同向型、异向型、啮合型、非啮合型中的任意一种;优选同向紧密啮合型双螺杆挤出机。
进一步的,所述的连接器为T型口模。
本实用新型的一种连续法生产热塑性聚氨酯弹性体的***,适合的TPU可以是任何类型的,如聚酯型TPU,聚醚型TPU,聚碳酸酯型TPU等类型。
采用本实用新型的***连续生产热塑性聚氨酯弹性体的方法,包括如下工艺步骤:
a前期混合和初期反应,将原料组分按比例计量,由浇注机浇注到挤出机第一加热区,调节挤出机转速和各区的加热温度,第一加热区温度为90℃,其余几个加热区温度为140-180℃,使物料进一步混合均匀,进行初期反应;
b后期反应和结晶,初期反应的物料通过连接器进入带式反应器,带式反应器前段加热,后期冷却,控制各区温度,在带式反应器中进行后期反应和结晶,加热段温度为80-210℃,冷却段温度稳定为70℃,在带式反应器内停留时间为8-30分钟,得到较高分子量的反应完全的片状物;
c成品,将片状物通过粉碎机粉碎,得到成品TPU颗粒,采用包装机进行包装。
热塑性聚氨酯弹性体的连续生产方法,由于生产热塑性聚氨酯弹性体的原料异氰酸酯、多元醇、扩链剂为界面反应,需要将三个完全接触才能够进行反应完全。挤出机机段主要是混合物料使物料初期反应,实际物料在此阶段反应程度较低,分子量还未达到需要的数值。因此此段控制温度主要是为了满足物料混合并初期反应的需要。根据TPU自身的反应特点,控制温度要保证物料在充分混合的同时能够引发反应,因此,挤出机机段第一加热区温度较低90℃左右;由于TPU为放热反应,所以后面几个加热区的温度达到140-180℃。因此挤出机提供高温反应,提供足够强的剪切,将TPU各组分混合和初期反应增链,物料的停留时间较短,小于1分钟,未完全反应的物料通过T型口模以一定厚度挤出在带式反应器上,在带加温功能的带式反应器上完成后期反应,流淌到带子上的片厚为1-10mm,在输送过程中将片材加热,加热段可采用热电偶加热,加热温度为80-210℃,冷却段可采用冷风进行冷却,温度稳定为70℃,TPU在带子上的加热时间为5-20分钟,冷却时间为3-10分钟,反应时间控制在8-30分钟,缓慢完成后期反应并且结晶,然后将冷却后的片材通过粉碎机粉碎,获得TPU粉碎颗粒。
本实用新型所述的一种连续法生产热塑性聚氨酯弹性体的***与已有技术相比具有如下积极效果,采用挤出机进行混合和初期反应,采用带控温功能的带式反应器进行后期反应和结晶,物料反应更加充分,相分离程度高,增加了产品结晶,提高了产品的拉伸强度和结晶温度,而且通过将反应分批进行,抑制了超大分子的生成,有效地降低了产品凝胶和不溶物,提高产品的使用范围,可以满足要求较高产品。
附图说明:
图1是本实用新型的连接示意图。
具体实施方式:
为了更好地理解与实施,下面结合附图给出具体实施例详细说明本实用新型。
本实用新型通过以下的实施例和对照例进行说明:
以下对照例和实施例采用的TPU配方:
二苯基甲烷 4,4’-二异氰酸酯(MDI)
32.6%(重量)
聚己二酸1,4丁二醇-酯(PBA,摩尔质量2000g/mol)
58.1%(重量)
1,4-丁二醇(BDO)(摩尔质量为90.123g/mol,官能度为2)
8.8%(重量)
催化剂:辛酸亚锡
0.011%(重量)
抗氧剂:Irganox®
1010
0.5%(重量)
对照例1,将存储于机械储料罐内的聚酯型多元醇(催化剂和抗氧剂直接加入到多元醇中),二异氰酸酯MDI(二苯基甲烷二异氰酸酯)(储存温度43℃),扩链剂BDO(1,4-丁二醇)(储存温度60℃),通过博雷浇注机浇注到挤出机的挤出机机段,混合头转速为3600RPM,控制挤出机机段第一加热区温度为180℃,其余几个加热区温度为200℃±5℃,螺杆转速控制为40Hz;通过水下造粒获得TPU颗粒。
对照例2,将存储于机械储料罐内的聚酯型多元醇(催化剂和抗氧剂直接加入到多元醇中),二异氰酸酯MDI(二苯基甲烷二异氰酸酯)预先混合通过管式反应器生成预聚物,然后同扩链剂BDO(1,4-丁二醇)由博雷浇注机浇注到挤出机的挤出机机段,混合头转速为3600RPM,控制挤出机机段第一加热区温度为180℃,其余几个加热区温度为200℃±5℃,螺杆转速控制为40Hz;通过水下造粒获得TPU颗粒。
实施例1,参见图1,根据原料储存量选择储料罐1,选择博雷浇注机2,选择长度为2320mm、直径为71mm、螺杆长径比L/D为32,有8个加热区的同向紧密啮合型双螺杆挤出机3,选择宽幅为1.2米的T型口模作为连接器7,选择长度为20米钢带或者采用聚四氟乙烯带、外加烘箱流道做为带式反应器4;同时选择常规的粉碎机5;将挤出机3和带式反应器4之间通过T型口模连接器7连接;最后通过包装机6进行包装,由上述设备组成本实用新型的***。
采用实施例1的***,将存储于储料罐内的聚酯型多元醇(催化剂和抗氧剂直接加入到多元醇中)、二异氰酸酯MDI(二苯基甲烷二异氰酸酯)和扩链剂BDO(1,4-丁二醇),用博雷浇注机浇注到挤出机的挤出机段,混合头转速为3600RPM,控制挤出机机段第一加热区温度为90℃,其余几个加热区温度为140℃-180℃,螺杆转速控制为40Hz;通过T型口模将TPU浇注在带式反应器上,浇注厚度为4mm,宽幅为1.2米的片材,烘箱流道内前5段加热,温度为130度,后面3区风冷降温,温度稳定为70度,在烘箱流道内停留时间为20分钟;最后将片材进行粉碎,获得TPU粉碎颗粒,通过包装机进行包装。
采用实施例1的***,将存储于储料罐内的聚酯型多元醇(催化剂和抗氧剂直接加入到多元醇中)、二异氰酸酯MDI(二苯基甲烷二异氰酸酯)和扩链剂BDO(1,4-丁二醇),用博雷浇注机浇注到挤出机的挤出机段,混合头转速为3600RPM,控制挤出机机段第一加热区温度为90℃,其余几个加热区温度为140℃-180℃,螺杆转速控制为40Hz;通过T型口模将TPU浇注在带式反应器上,浇注厚度为1mm,宽幅为1.2米的片材,烘箱流道内前5段加热,温度为80度,后面3区风冷降温,温度稳定为70度,在烘箱流道内停留时间为8分钟;最后将片材进行粉碎,获得TPU粉碎颗粒,通过包装机进行包装。
采用实施例1的***,将存储于储料罐内的聚酯型多元醇(催化剂和抗氧剂直接加入到多元醇中)、二异氰酸酯MDI(二苯基甲烷二异氰酸酯)和扩链剂BDO(1,4-丁二醇),用博雷浇注机浇注到挤出机的挤出机段,混合头转速为3600RPM,控制挤出机机段第一加热区温度为90℃,其余几个加热区温度为140℃-180℃,螺杆转速控制为40Hz;通过T型口模将TPU浇注在带式反应器上,浇注厚度为10mm,宽幅为1.2米的片材,烘箱流道内前5段加热,温度为210度,后面3区风冷降温,温度稳定为70度,在烘箱流道内停留时间为30分钟;最后将片材进行粉碎,获得TPU粉碎颗粒,通过包装机进行包装。
将上述实施例和对照例生产的TPU产品物性进行了对比,结果见表1。
表1
上述,薄膜凝胶通过以下方式进行判定:将TPU颗粒物料在直径为30mm单螺杆挤出机熔化并通过T型口模挤出4.5-6厘米宽,6-10毫米厚的薄膜长条。
压缩变形通过ASTMD395 B法进行测试,测试样条为直径为13mm,6mm的圆柱。在控温70℃,放置22小时,压缩25%℃的条件下进行测试。
由以上结果可以看出,采用挤出机和带式反应器的***生产的产品能够提高强度,有效降低产品凝胶,扩大产品使用范围。
Claims (3)
1.一种连续法生产热塑性聚氨酯弹性体的***,其特征在于它包括储料罐(1)、浇注机(2)、挤出机(3)、带式反应器(4)、粉碎机(5)和包装机(6),所述挤出机(3)和带式反应器(4)之间通过连接器(7)连接;所述挤出机(3)为双螺杆挤出机或单螺杆挤出机;所述带式反应器(4)为带加温功能的钢带或者聚四氟乙烯带。
2.根据权利要求1所述的一种连续法生产热塑性聚氨酯弹性体的***,其特征在于所述的双螺杆挤出机螺杆类型为同向啮合型。
3.根据权利要求1所述的一种连续法生产热塑性聚氨酯弹性体的***,其特征在于所述的连接器为T型口模。
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