CN107708972B - 酚醛树脂的方法 - Google Patents

酚醛树脂的方法 Download PDF

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CN107708972B
CN107708972B CN201680029227.6A CN201680029227A CN107708972B CN 107708972 B CN107708972 B CN 107708972B CN 201680029227 A CN201680029227 A CN 201680029227A CN 107708972 B CN107708972 B CN 107708972B
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CN107708972A (zh
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丹尼尔·巩特尔
弗洛里安·莫格勒
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Abstract

本发明涉及一种使用分层技术生产组件(103)的方法、装置、粘结剂体系(400)和材料体系，其中施工空间和/或施加的材料中的温度被设定为至少70℃并保持至少2小时，并且其中已选择性地施加粘合剂(400)的区域固化并形成组件(103)。

Description

酚醛树脂的方法
技术领域
本发明涉及一种用于制造三维组件的方法和装置。这些模制组件适合于在铸件应用中使用，特别是作为模具和型芯。
背景技术
欧洲专利EP 0431924B1描述了一种基于计算机数据生产三维物件的方法。在此方法中，在平台上沉积一层薄的颗粒材料，并在其上通过打印头选择性地印刷粘合剂材料。其上印有粘合剂的颗粒区域在粘合剂和任选的额外的硬化剂的影响下粘合并固化。接下来，将平台降低一个层厚度进入到施工圆筒中，并提供新的颗粒材料层，后者也如上所述被印刷。重复这些步骤直到达到物件的某个所需的高度。因此，印刷和固化后的区域形成三维物件(组件)。
完成后，把由固化的颗粒材料制成的物件嵌入在松散的颗粒材料中，随后从该松散的颗粒材料中释放出来。为此，例如可以使用抽吸装置。这留下了所需的物件，其随后必须没有任何残留的粉末，例如通过刷掉粉末。
在已知的方法中，对于使用的粘合剂会出现问题，这些粘合剂经常物理攻击装置本身，特别是打印头，并且在某些情况下，在健康方面也是有问题的。
而且，进一步的工艺条件对于有利的组件的生产可能是有问题的并且是次优的。特别是，温度分布和合适的粘合剂并不总是允许积极的工艺结果，并经常对经济可行性产生不利影响。
因此，本发明的一个目的是提供一种方法，通过该方法可以生产有利的组件，并且在经济可行性方面是有利的，或者至少避免或者至少减少了现有技术的缺点。
发明内容
本发明所述的是一种组件的分层施工的方法，其中将颗粒材料按层厚度逐层施加到施工空间中的施工区域上，选择性地施加粘合剂，施工空间中和/或施加的颗粒材料中的温度被调节至所需的温度，并且重复施加材料和施加粘合剂的步骤，直到获得所需的组件；其中，将施工空间中和/或施加的材料中的温度调节至至少70℃并保持至少2小时，选择性施加粘合剂的区域固化并形成所述组件。
在这种情况下，有利的是可以使用没有问题的粘合剂体系，其基于水性溶剂或醇类溶剂，并且其可在很长一段时间内被调节并保持在施加的颗粒材料中的至少70℃的温度。使用这样的方法具有这样的优点：因此，施加的颗粒材料中的非常大的区域保持均匀的所需温度，这反过来允许获得均匀的固化并获得有利的组件特性。这不仅具有在组件中获得均匀的材料特性的优点，而且有利地可以使用施工空间的大区域来制造组件，并且保持相对小的具有颗粒材料的施工空间的未使用的边缘区域。这提高了装置的效率，并由此分别降低了每个组件或高容量组件的成本。在该方法中使用的粘合剂体系优选在室温下仅具有轻微的反应性，并且机械组件特别是打印头易于清洁并且允许维护而没有任何显著的问题。
附图说明
图1表示基于粉末的3D打印机的组件的斜向剖视示意图。
图2表示使用逐层辐射固化的常规3D印刷工艺的顺序示意图。
图3表示包括在每层中不受影响的辐射固化的施工工艺的顺序示意图。
图4表示将粘合剂(400)施加到所提供的颗粒材料上的示意图，其中(401)代表一个颗粒，黑色箭头表示渗透的方向。在这种情况下，组件的强度通过粘合剂粘合颗粒材料的颗粒和所发生的粘合剂的固化而获得，这导致粘合剂与颗粒材料的固体连接。图4a-4d描述了粘合剂渗入颗粒材料的顺序。
图5中的图5a和5b分别示出能量输入/热量输入(500，501，502)和能量损失/热量损失(503，504，505)。图5c显示非常不均匀的温度分布，在这种情况下，在其中发生固化反应的等温线(510-514)朝向远离施工容器的中心移动。这大大减少了有用的施工空间，并且装置和方法的经济可行性是不利的。图5c示出了本发明所公开的方法中的一种情况，并且变得明显的是，有用的施工空间或有用的施加的粉饼均分别是较大的，这导致机器的经济可行性的提高，同时，该组件可是有利的。这由等温线510表示，该等温线包括在该工艺期间保持温度均匀的大区域，因此获得积极的工艺结果。
图6表示如由可溶性酚醛树脂举例说明的预聚物的制备的示意图。
图7表示可溶性酚醛树脂与交联树脂的缩合反应的示意图。
附图标记列表
100 喷墨打印头
101 粉末涂覆机
102 施工平台
103 组件
104 施工场地边缘
107 粉末层
200 热源
300 用于容器壁的电阻加热/液体加热/加热
301 用于施工平台的电阻加热/液体加热/空气加热
302 热风机
303 静态加热器
304 具有接触元件的电阻加热
400 粘合剂/粘合剂体系
401 粉末颗粒
500 施工场地表面的能量输入
501 通过施工容器壁进入粉饼的能量输入
502 通过施工平台进入粉饼的能量输入
503 施工场地表面的能量损失
504 通过施工容器壁的粉饼的能量损失
505 通过施工平台的粉饼的能量损失
510 粉饼中的等温线为90℃
511 粉饼中的等温线为80℃
512 粉饼中的等温线为70℃
513 粉饼中的等温线为60℃。
具体实施方式
在下文中，将更精确地定义几个术语。否则，所使用的术语将具有本领域技术人员已知的含义。
就本发明而言，“3D打印方法”是现有技术中已知的所有方法，其能够在三维模具中施工组件并且与所描述的工艺组件和装置兼容。特别地，这些方法包括基于粉末的方法，其含有作为一种成分的水溶液或/和其它流体成分或溶剂，这些成分或溶剂必须从模制组件中除去或在固化过程中从模制组件中逸出。本发明可以选择性地影响模制组件的固化和质量，其他质量特征保持不变或甚至受到正面影响。
本发明意义上的“模制组件”，“模型”，“3D模制组件”或“组件”是指通过根据本发明的方法或/和根据本发明的装置制造的所有三维物件，其表现出尺寸稳定性。
用于实施根据本发明的方法的“装置”可以是包括所需组件的任何已知的3D打印装置。常见的组件包括涂覆器、施工场地、用于施工场地或其他组件的装置、剂量装置、打印头、加热介质、用于分批式或连续式工艺的位移装置，以及本领域技术人员已知的其他组件将，因此不在此详细描述。
根据本发明，“施工平台”或“施工区域”相对于印刷和涂覆机的水平方向移动。这种相对运动是在施工工艺中发生，其达到层厚度时中断运动。运动限定了层厚度。作为替代，装置可以被构造成使得装置的其他部分向上移动，由此调整层强度或层厚度。
“施工容器”或“作业箱”提供了一个施工空间。因此，该施工空间有底部，墙壁和开口进入区域。施工容器总是包括相对于3D打印装置的框架不移动的组件。可更换的施工容器(称为作业箱)允许机器实际上持续运行，因为作业箱可以移入和移出机器。因此，第一次施工操作的组件可以在设备(3D打印设备)外部拆开，而新的组件已经可以在机器内的第二个施工容器中被印刷。
本发明的意义上的“施工空间”是指一几何位置，在该几何位置处，由颗粒材料的重复涂覆的施工工艺期间颗粒材料层进行生长。施工空间通常由底部(即施工平台)、墙壁和开口顶部表面(即施工平面)限定。施工平面可以是水平的，但是也可以例如在连续工艺中形成角度，从而以倾斜的角度进行涂覆。
这里使用的“颗粒材料”或“施工材料”或“颗粒物”可以是已知用于基于粉末的3D打印的任何材料，特别是砂、陶瓷粉末、金属粉末、塑料材料、木材颗粒、纤维材料、纤维素或/和乳糖粉末。颗粒材料优选在干燥时能自由流动的粉末，但也可以使用具有粘合力的耐切割粉末。在一个优选的方面，所使用的颗粒材料可以被认为是“被动粉末材料”，因为它不直接参与组分的结合反应，即固化，而是仅被粘合剂体系固化或“连接”成一个固体组件。它可能会显示惰性行为。所施加的颗粒材料也可以被称为粉饼。
“调节温度”或“回火”是指在施工空间或/和施加的颗粒材料中调节至特定的温度，或者将施工空间调节到选定的温度。在一个方面中，特别地，所施加的颗粒材料被回火，并且温度保持在例如约60℃、70℃、80℃、90℃、100℃、110℃、120℃、130℃、140℃、150℃或者保持在80℃至100℃。
“粘合剂”或“粘合剂体系”是通过打印头选择性地施加到颗粒材料上的材料，并且该材料导致固化并因此生产组件。粘合剂体系包含溶剂和其它组分，例如，单体、低聚物和/或聚合物。结合机理是聚合反应。其结果是一固体材料，该固体材料能够结合粉末中的颗粒。作为基础材料，预聚合酚醛树脂是优选的。
“扩散长度”对应于在颗粒材料中施加的粘合剂的膨胀性，并且尤其受到粘合剂的体积、温度和组成的影响。
下面将描述优选实施例。
本发明所公开的是一种组件的分层施工的方法，其中将颗粒材料按层厚度逐层施加到施工空间中的施工区域上，选择性地施加粘合剂，施工空间中和/或施加的颗粒材料中的温度被调节至所需的温度，并且重复施加材料和施加粘合剂的步骤，直到获得所需的组件；其中，将施工空间中和/或施加的材料中的温度调节至至少70℃并保持至少2小时，选择性施加粘合剂的区域固化并形成所述组件。
使用本文公开的方法，组件被生产，一方面所述组件显示出阳性材料的性质，另一方面，所公开的方法允许增加所施加的粉饼内的有效空间，这是因为可以调整和维持在反应所持续的时间内所必需的恒定的温度。
选择温度以使得在粉饼中，具有阳性组分性质的固化所需的反应温度被设定为是均匀的。优选将温度调节为70～90℃，优选为80℃以上，更优选为90℃以上，进一步优选为80～150℃，进一步优选为80～100℃。这也被称为等温线，优选80℃的等温线，优选90℃的等温线。
以这种方式，在粉饼的有利的大区域中，即在施加的颗粒材料的区域中，基本均匀的温度被调整并保持。
在该方法中，温度被保持在反应所需的时间内，优选3至10小时，更优选4至6小时，并且更优选至少4小时。
可以使用本领域技术人员已知的任何合适的颗粒材料，颗粒材料优选为塑料材料、砂、陶瓷材料或金属。在这种情况下，粒度可以根据需要与其他工艺参数的相互作用进行选择。平均粒径优选为8μm以上，更优选为10μm～1mm。
颗粒材料可以以不同的层厚度施加，优选50～800μm的层厚度。
粘合剂适用于其它工艺材料和条件，并且所使用的粘合剂可以优选为一粘合剂体系，所述粘合剂体系包含单体、低聚物或/和聚合物以及溶剂，所述溶剂优选为水性溶剂或醇类溶剂。
通过该方法获得的组件优选具有至少280N/cm2的组件生坯强度。
该方法允许组件的最终强度(弯曲强度)为至少300N/cm2，优选至少500N/cm2，该最终强度可直接或者在进一步的处理步骤之后实现。
在该方法中，设定工艺条件，以使得由此产生的组件的烧失量小于3％，优选小于2.5％，更优选小于2.2％。
进一步的处理步骤是可能的，所得到的组件可以经受进一步的处理步骤。
另一方面，本发明涉及一种粘合剂体系，所述粘合剂体系包含单体、低聚物或/和聚合物以及溶剂，所述溶剂优选为水性溶剂或醇类溶剂。所述粘合剂体系包含预聚合酚醛树脂。
另一方面，本发明涉及一种包含如上所述的颗粒材料和如上所述的粘合剂体系的材料体系。
另一方面，本发明涉及一种用于生产组件的装置，所述装置包括具有施工平台的施工空间，用于施加颗粒材料的设备，用于选择性地施加粘合剂体系的设备，用于调节施工空间中或/和颗粒材料中的温度的设备。下面将更详细地介绍本发明的其他方面，并且这些设备元件可以以期望的任何有用的和功能性的方式进行相互组合。
最后，另一方面，本发明涉及一固体(组件)，该固体由如本文所述的方法、粘合剂体系、材料体系或/和装置生产，其中所述固体优选具有弯曲500N/cm2的弯曲强度。
下面将描述其他方面。
所述方法的一个方面是粘合剂体系或粘合剂(400)，其印刷在对反应呈中性的粉末(401)上，并在数小时内在比室温高得多的温度下固化。所述固化的大部分在施工工艺中发生。在这种情况下，整个所得到的粉饼保温几个小时。
可以使用各种颗粒材料(401)作为粉末。这包括陶瓷粉末、砂甚至金属粉末。对于该方法，粉末颗粒(401)实质上不应当小于10μm。大于1mm的颗粒(401)通常使安全加工困难。这些说明是指平均粒度。然而，即使满足平均粒径要求，上述最大和最小颗粒(401)的相当大的一部分也不利于该加工。
通过与施工平台(102)一起的涂覆机(101)将颗粒在装置中加工成薄层(107)。为此目的，颗粒材料(401)在起始位置或从起始位置供应，并且通过在施工场地上移动的涂覆机(101)进行平滑。施工平台的相应位置决定了层厚度。
在根据本发明的树脂体系或粘合剂(400)中，粉饼被保持在80℃的温度下至少4小时。这导致组件的弯曲强度超过300N/cm2，烧失量小于2.2％。
粘合剂体系(400)包括作为结合成分的单体、低聚物和/或聚合物。这些在溶剂中溶解。结合机理是聚合反应。它产生了能够结合粉末中的颗粒的固体材料。作为基础材料，预聚合酚醛树脂是优选的。
根据本发明，粘合剂体系(400)被配置以用于包括压电元件的喷墨打印头(100)。在这种情况下，其粘度范围为5至20mPas。室温下蒸汽压力小于3000Pa。表面张力在30-50mN/m的范围内。粘合剂体系被调整，以使得至少需要约1分钟可逆地干燥打印头以阻止第一次喷射的作用。
粘合剂体系(400)在室温下表现出极低的反应性。这保护了打印头(100)，即使在长使用寿命之后，打印头仍保持高度可靠性。即使在数周之后，干燥的粘合剂也容易在室温下除去。这有利于设备的清洁和干燥喷射的重新激活。
在酚醛树脂的情况下，用于粘合剂体系的溶剂可以是水。因此，如果处理得当，粘合剂体系可以被认为是无害的。
由于热的施工场地表面的热效应，打印头(100)被主动地或被动地冷却，因此从而允许在整个施工工艺中，滴落量和输出量保持恒定。通过与打印头清洁单元连接可以实现被动冷却。主动冷却可以例如通过冷却水流过并且安装到打印头(100)的冷却元件来实现。预冷的压缩空气的引入，以及一个风扇均适合用于冷却。
当到达颗粒材料的表面时，根据表面张力的函数，由打印头(100)打印的粘合剂缓慢地渗入粉饼中。在这种情况下，需要一定的扩散长度。所述扩散对于将各个层彼此结合是必需的。扩散长度取决于流体参数，也取决于施工场地的温度。此外，在施工工艺中温度受到控制，印刷层慢慢固化，因此可以进行层间粘合。
例如，如果使用水作为溶剂，则在低于100℃下工作是有利的。在此限度以上，会出现蒸发效应，这可能对组件的表面质量产生不利影响。
该方法将扩散长度设定为层厚度的1.5倍是有利的。这导致在结构方向上的各向异性，组件的底面的分辨率和质量之间的良好折衷。
在这个过程中，50-800μm的层厚度是可能的且有用的。层厚度根据粉末材料和所需的施工进度进行调整。
该装置包括用于加热粉饼并保持其温度的装置(200，300-304)。在这种情况下，能量输入可以部分地被粉末绝缘，使得一旦被加热的粉末不能被快速冷却。
可以使用红外热源作为加热装置。它们可以静态布置(302)在施工场地之上或者通过装置的移动部分在施工场地上移动(200)。由石英玻璃制成的卤素辐射器以及陶瓷辐射器都是合适的。红外辐射镜也适用于影响和控制热平衡。
例如，最大功率为9.5kW、长度为1米的器的红外辐射可用于加热100×60cm的施工场地。在这种情况下，散热器在施工场地例如以0.05m/s的速度来回移动。这个过程通常与涂覆工艺相结合。对于约为60秒的涂覆时间约，在进行施工工艺期间，粉饼中的温度可能超过90℃，这基本上是由印刷和辐照导致。作为替代方案，除了所描述的照射和/或作为唯一的加热程序，可以使用每n层进行x次单独的辐照通道，n≥2，优选每2至5层，特别优选每3层，并且x≥1次辐照，优选2至5次，特别优选3至4次辐照。
而且，热空气可能在施工场地上扫过(301)，从而加热它。所有形式的热风机(301)都适用于此目的。用气流或电阻加热直接预热粉末也是可能的。而且，接触式的加热的金属可在粉末(304)上被引导以将其加热。
另一种合适的工艺装置是在施工容器壁(300)和/或施工平台(301)中进行加热。一方面，这些可以给工艺过程带来热量；另一方面通过主动隔热，可以减少热量损失。
这种加热例如作为电阻加热可以被提供。他们可以通过标准的控制设备进行控制。为此目的，通常使用例如可以粘合到金属表面(例如施工容器壁)上的片材。通过***金属板孔中的加热筒来提供相同的效果。
在隔热不良的情况下，对于高达约90℃的温度，需要输出功率可达5W/cm2。。根据隔热性能的不同，这里可以节省大量的能源。
此外，主动隔热可以使用传热介质实现。传热介质(例如水或油)可以在通常由铜制成的管中输送，以接触的方式在作业箱壁和作业箱底板内延伸并且优选地以曲折的方式延伸以实现作业箱的可能的最均匀的加热。
被动隔热对施工容器中的温度控制也是有用的。在这种情况下，可以使用不同的“材料”，例如在建筑行业中常见的“材料”：矿物隔热材料，塑料材料，泡沫材料，还有空气，真空等。被动隔热材料被安装以使得来自施工容器的热流动减少。
该装置的另一个重要设备是其控制单元。控制单元确定装置内的温度控制。为此目的，用于检测重要温度参数的设备可以存在于装置中。这允许提供控制电路。一个简单的变体是控制输入到装置的功率。在这种情况下，在机器的预热阶段发生较高的功率输入。正在进行的工艺过程中，功率逐渐降低。
在上述具有9.5kW辐射器的装置中，例如，在施工工艺的前3个小时期间，功率从100％降低到70％。有了这个动力，整个过程在达到静止状态之后进行。
加热元件和隔热件的组合必须相互适应以在粉饼中实现均匀的温度场(例如图5d)。所需的均匀性取决于粘合剂体系。为了确保粘合剂的可靠固化，必须超过一明确的特定的阈值。
一般来说，选定的温度不能太高，否则印刷和施工工艺会受到影响。这里施工场地的表面温度不应该超过90℃。为了达到足够的强度，温度必须高于80℃。换句话说，温度必须在10K范围内。
如果温度分布变得非常不均匀(图5c)，在其中发生固化反应的等温线(510-514)朝向远离施工容器的中心移动。这大大减少了有用的施工空间。
粘合剂体系是可热固化的预聚合酚醛树脂溶液和/或酚醛清漆溶液，其在已经描述的条件下在施工工艺中部分或完全地反应成不溶和不熔融的树脂。整个施工工艺中的温度控制被选择，以使得固化不会立即发生，但在几个小时的时间内，允许层间粘合。(图7)
酚醛树脂和酚醛清漆是苯酚-甲醛共缩合物的预聚物。酚醛树脂是在碱性条件下用过量的甲醛与苯酚聚合的预聚物。(图6)
酚醛树脂包括数量增加的游离羟基，其在温度影响下趋于进一步缩聚并形成不溶性酚醛树脂。
酚醛清漆是在甲醛不足的酸性条件下合成的预聚物，并在温度影响下与可溶性酚醛树脂共缩合形成不熔酚醛树脂，或在温度升高下与添加的甲醛供体(例如乌洛托品)聚合。
由于其生产过程，预聚物含有苯酚和甲醛的残余单体。苯酚含量优选低于5％，特别优选低于1％。
甲醛含量优选低于0.3％，特别优选低于0.1％。
通过加入由单醇和/或多元醇和/或水或仅由水组成的溶剂，将粘合剂分别稀释或调节至粘度在5-20mPa·s范围内，优选在5-10mPa·s，特别优选5-8mPa·s。
为了粘度的精确调整，可以使用其它改性剂，例如多价醇如乙二醇，丙二醇或丙烯甘醇，进一步地如羧甲基纤维素，木糖醇，山梨醇或***树胶。优选使用1％-9％，特别优选3％-7％。
为了调整表面张力，可以使用普通的表面活性剂，例如十二烷基硫酸钠或月桂醇醚硫酸钠以及含氟和硅氧烷基表面活性剂。
粘合剂液体通常由30％-40％预聚物，60％-70％溶剂和1％-7％粘度改性剂组成。
根据所需的最终强度和烧失量，粘合剂的投入量可以在很宽的范围内调节。通常，选择投入量和温度控制，使生坯强度不低于280N/cm2，以确保组件的安全运转。如果在施工工艺中缩合反应未完全达到，则后续的烘箱过程可以完成反应。优选地，随后将组分在120℃-150℃下烘焙1-4小时，特别优选在130℃-140℃下烘焙2-3小时。任何残留的溶剂仍然会被这个操作完全排出。
通常，使用颗粒材料的5wt％-8wt％的投入量，这使得可获得足够的生坯强度和高的最终强度。
这些例子以优选实施例进行描述，而不被解释为限制性的。
实施例
实施例1
粘合剂混合物：可溶性酚醛树脂/酚醛清漆预聚物35％，水/异丙醇(80/20)63％，1,2-丙二醇3％；
投入量：5.8wt％；
颗粒物质：AFS 100硅砂；
生坯强度：380N/cm2；
最终强度：540N/cm2(在135℃下3小时后)；
烧失量：2％。

Claims (6)

1.一种组件的分层施工的方法，其特征在于，将颗粒材料按层厚度逐层施加到施工空间中的施工区域上，选择性地施加粘合剂，施工空间中和/或施加的颗粒材料中的温度被调节至所需的温度，并且重复施加材料和施加粘合剂的步骤，直到获得所需的组件；其中，将施工空间中和/或施加的材料中的温度调节至80至90℃并保持至少2小时，选择性施加粘合剂的区域固化并形成所述组件；
其中，在施加颗粒材料的区域中，调节并保持一基本上均匀的温度；
其中，所述温度被保持3至10小时；
其中，所述颗粒材料是塑料材料、砂、陶瓷材料或金属；或/和
所述颗粒材料的平均粒径为至少为8μm；或/和
所述层厚度为50～800μm。
2.根据权利要求1所述的方法，其特征在于，所使用的粘合剂是一粘合剂体系，所述粘合剂体系包含单体、聚合物以及溶剂，所述溶剂为水性溶剂或醇类溶剂。
3.根据权利要求1所述的方法，其特征在于，所述组件的生坯强度为至少280N/cm2。
4.根据权利要求1所述的方法，其特征在于，所述组件的最终弯曲强度为至少300N/cm2。
5.根据权利要求1所述的方法，其特征在于，所生产的组件的烧失量小于3％。
6.根据权利要求1所述的方法，其特征在于，所获得的组件经受进一步的处理步骤。
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US20210016500A1 (en) 2021-01-21
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