CN110436945B - 用于注射模塑组合物的粘合剂 - Google Patents

用于注射模塑组合物的粘合剂 Download PDF

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CN110436945B
CN110436945B CN201910347902.5A CN201910347902A CN110436945B CN 110436945 B CN110436945 B CN 110436945B CN 201910347902 A CN201910347902 A CN 201910347902A CN 110436945 B CN110436945 B CN 110436945B
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binder
volume
ethylene
powder
copolymer
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CN110436945A (zh
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D·卡蒂尔
J·迪迈
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Comadur SA
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Comadur SA
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    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
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Abstract

本发明还涉及用于注射模塑组合物的粘合剂，其包括：‑40至55体积％的聚合物基料，‑35至45体积％的蜡混合物或蜡和棕榈油的混合物，‑和至少5体积％的至少一种表面活性剂，其中所述聚合物基料由乙烯与甲基丙烯酸或丙烯酸的共聚物、乙烯与丙烯的共聚物和/或马来酸酐接枝的聚丙烯，和可溶于异丙醇、丙醇和/或松节油并选自乙酸丁酸纤维素、聚乙烯醇缩丁醛和共聚酰胺的聚合物形成，粘合剂组分各自的量使得它们的总和等于100体积％的粘合剂。

Description

用于注射模塑组合物的粘合剂
技术领域
本发明涉及用于注射模塑的粘合剂组合物和意图用于制造成型金属或陶瓷部件的注射模塑组合物(原料)。
背景技术
在用于首饰和钟表工业或甚至用于技术用途，如医疗设备、电子学、电话学、工具、机械切削刀片、消费品行业的硬质材料的制造中，尤其是对于通常指定在无机“陶瓷”的类属名下的硬质材料，实施粉末冶金技术。所得合成无机材料在此被称为“陶瓷”，无论该材料的性质如何，是蓝宝石、红宝石、人造金刚石、蓝宝石玻璃、陶瓷、微磁体、金属、合金还是其它。
一般而言，基础原材料的性质不同并且至少包括，一方面，陶瓷粉末，另一方面，有机粘合剂，如树脂或塑料或类似物，它们使得能够注射用所有原材料的混合物制成的组件并实现良好耐受性。在该混合物中可包括其它添加剂。这些原材料也可能具有不同质地：固体、粉末、液体或糊。该混合物的结构也可能在其制造过程中改变，特别但不限于，当树脂的互补组分发生聚合反应时。
无机陶瓷组件的整个制造方法包括至少下列步骤：
-制备原材料(raw materials)；
-混合原材料，或/和如果需要，两两(或更多)预混；
-均化；
-造粒；
-压制，尤其在压制室中压制一定量的获自均化和造粒步骤的粉末或原料(feedstock)丸粒，以制造被称为“生坯件(green part)”的坯体。该压制操作可以通过在压力下(尤其在包括加热所述量的获自均化或造粒步骤的粉末或原料丸粒的装置的螺杆注射器中)注射模塑进行；
-用于燃烧该混合物的某些成分的温度受控脱脂(debinding)(热脱脂)和/或在合适的溶剂中溶解该混合物的某些成分(溶剂脱脂)；
-在脱脂后热处理生坯件，用于二次热脱脂工艺和烧结，这赋予成品组件最终内聚力。这种热处理造成尺寸收缩，从而能够获得具有最终尺寸的组件，
-该组件的表面精加工处理。
本发明的一个特定目的是为注射模塑组合物提供优化的粘合剂，其促进粉末冶金混合以获得陶瓷或金属，从而获得具有受控收缩系数的质量高度可再现的产品。
例如申请人的专利申请No.WO 2014/191304是已知的，其公开了用于制造模制陶瓷或金属部件的注射模塑组合物(原料)，其含有烧结的无机粉末和有机粘合剂，后者基本由乙烯和甲基丙烯酸的共聚物、聚乙烯、聚丙烯、丙烯酸系树脂和蜡的混合物形成。
这些原料具有许多优点。更特别地，它们提供良好的均匀性和良好的流动性，以允许制造更复杂形状的金属或陶瓷部件。它们也提高生坯件和粘合剂对生产应力(加工(handling)和各种精加工(finishing)操作)的机械耐受性，并有可能使用可通过简单热处理清除的无污染溶剂实施溶剂脱脂，以除去一部分有机粘合剂。
发明内容
发明概述
本发明的一个目的是通过提出用于进一步改进注射组合物的粘度的新型原料来克服上述缺点，以获得更高效的溶剂脱脂和获得美学质量改进的组件。
本发明因此涉及一种用于注射模塑组合物的粘合剂，其包括：
-40至55体积％的聚合物基料，
-35至45体积％的蜡混合物或蜡和棕榈油的混合物，
-和至少5体积％的至少一种表面活性剂，
其中所述聚合物基料由乙烯与甲基丙烯酸或丙烯酸的共聚物、乙烯与丙烯的共聚物和/或马来酸酐接枝的聚丙烯，和可溶于选自异丙醇、丙醇、松节油及其混合物的溶剂并选自乙酸丁酸纤维素、聚乙烯醇缩丁醛和共聚酰胺的聚合物形成，粘合剂组分各自的量使得它们的总和等于100体积％的粘合剂。
本发明还涉及意图用于制造成型金属或陶瓷部件的注射模塑组合物(原料)，其包括76至96重量％的无机粉末和4至24重量％的上文定义的粘合剂。
根据本发明的注射模塑组合物能够改进注射组合物的粘度，获得更高效的溶剂脱脂和获得美学质量改进的组件。
具体实施方式
优选实施方案详述
根据本发明，用于注射模塑组合物的粘合剂包括下列组分：
-40至55体积％，优选45至54体积％的聚合物基料，
-35至45体积％，优选39至42体积％的蜡混合物或蜡和棕榈油的混合物，
-和至少5体积％，优选5至15体积％的至少一种表面活性剂，
其中所述聚合物基料由乙烯与甲基丙烯酸或丙烯酸的共聚物、乙烯与丙烯的共聚物和/或马来酸酐接枝的聚丙烯，和可溶于异丙醇和/或丙醇和/或松节油并选自乙酸丁酸纤维素、聚乙烯醇缩丁醛和共聚酰胺的聚合物形成，粘合剂组分各自的量使得它们的总和等于100体积％的粘合剂。
优选地，本发明的粘合剂的聚合物基料包括2至7体积％的乙烯与甲基丙烯酸或丙烯酸的共聚物、0至40体积％的乙烯与丙烯的共聚物、0至35体积％的马来酸酐接枝的聚丙烯(乙烯与丙烯的共聚物和马来酸酐接枝的聚丙烯的总量在30至40体积％之间)，和6至15体积％的可溶于异丙醇和/或丙醇和/或松节油的聚合物，至100体积％的粘合剂，粘合剂组分各自的量使得它们的总和等于100体积％的粘合剂。
优选地，该聚合物基料包括乙烯与丙烯的共聚物和马来酸酐接枝的聚丙烯的混合物。
优选地，本发明的粘合剂的聚合物基料包括2至7体积％的乙烯与甲基丙烯酸或丙烯酸的共聚物、25至30体积％的乙烯与丙烯的共聚物、5至10体积％的马来酸酐接枝的聚丙烯和6至15体积％的可溶于异丙醇和/或丙醇和/或松节油的聚合物，至100体积％的粘合剂。
更优选地，本发明的粘合剂的聚合物基料包括3至5体积％的乙烯与甲基丙烯酸或丙烯酸的共聚物、26至29体积％的乙烯与丙烯的共聚物、6至8体积％的马来酸酐接枝的聚丙烯和6至12体积％的可溶于异丙醇和/或丙醇和/或松节油的聚合物，至100体积％的粘合剂。
优选地，该乙烯-丙烯共聚物是熔点在140℃至150℃之间的(无规)统计乙烯-丙烯共聚物，该熔点随所述共聚物中的乙烯和丙烯的百分比而变。例如，对于氧化物和氮化物粉末，该统计乙烯-丙烯共聚物优选含有更多丙烯以具有大约147℃的熔点。对于金属粉末，该统计乙烯-丙烯共聚物优选含有更多乙烯以具有大约140℃的熔点。
优选地，乙烯与甲基丙烯酸或丙烯酸的共聚物含有3至10重量％的甲基丙烯酸或丙烯酸系共聚单体。
优选地，马来酸酐接枝的聚丙烯具有1％至2％的接枝率和100℃至140℃的熔点。
优选地，可溶于异丙醇和/或丙醇和/或松节油的聚合物是具有相对于聚合物重量计37重量％至53重量％的丁酰基含量、2重量％至13重量％的乙酰基含量、125℃至165℃的熔点和16000至40000的分子量的乙酸丁酸纤维素。
有利地，该蜡是巴西棕榈蜡(Carnauba wax)或石蜡或这些成分的混合物。当该蜡与棕榈油混合时，该蜡优选是巴西棕榈蜡。
根据另一优选特征，表面活性剂是N,N'-亚乙基双硬脂酰胺，或硬脂酸和棕榈酸的混合物(stearin)，或这些成分的混合物。
根据另一特征，表面活性剂可溶于异丙醇和/或丙醇和/或松节油。
本发明还涉及意图用于制造成型金属或陶瓷部件的注射模塑组合物(原料)，其包括76至96重量％的无机粉末和4至24重量％的上文定义的粘合剂。
根据一个特定特征，该注射模塑组合物的无机粉末可选自氧化物粉末、氮化物粉末、碳化物粉末、金属粉末或所述粉末的混合物，该无机粉末优选选自氧化铝粉末、氧化锆粉末、碳化铬粉末、碳化钛粉末或碳化钨粉末、金属钨粉末或氮化硅粉末、不锈钢粉末、金属钛粉末或所述粉末的混合物。
根据注射模塑组合物的优选实施方案，该注射模塑组合物含有按重量％计：
·76至88％的氧化铝和12至24％的如上定义的根据本发明的粘合剂，或
·76至88％的氧化铝和0.1至0.6％的氧化镁和12至24％的本发明的粘合剂，或
·58至86.5％的氧化锆和3.9至4.6％的氧化钇和0.18至18.5％的氧化铝和9至22％的本发明的粘合剂，或
·61.5至84％的氧化锆和3.9至4.6％的氧化钇和0.2至9％的氧化铝和2至5.5％的选自氧化铁、氧化钴、氧化铬、氧化钛、氧化锰、氧化锌或所述氧化物的混合物的无机颜料和9至22％的本发明的粘合剂，或
·88至91％的铬或钛碳化物，和9至12％的本发明的粘合剂，或
·93至96％的碳化钨或金属钨和4至7％的本发明的粘合剂，或
·78至85％的氮化硅和15至22％的本发明的粘合剂。
根据本发明的意图用于制造成型金属或陶瓷部件的注射模塑组合物(原料)在同等剪切速率具有比已知原料低的粘度。因此，本发明的组合物能够在注射模塑过程中更好地填充部件，尤其是在薄壁区域中。此外，根据本发明的组合物使得部件的更高效溶剂脱脂成为可能，特别是通过改进的在异丙醇和/或丙醇和/或松节油溶剂中的粘合剂组分的清除。沸点为97℃的丙醇能够在更高温度下脱脂以改进效率，尤其是通过改进巴西棕榈蜡(熔点82℃)的清除。
本发明的组合物还能够获得具有改进的表面外观、没有可见裂缝或焊接线的模制和烧结部件。
现在借助下列非限制性实施例更详细例示本发明。
实施例
在大约150℃的温度下将粘合剂的聚合物部分与无机粉末混合以制造预混物。向所述预混物中加入蜡和表面活性剂，并将该温度进一步提高到大约180℃以形成一种均匀糊料，然后将其冷却并造粒至凝固，然后保存以形成可用于通过已知的注射模塑技术制造成型部件的原料。
该技术通常包括在具有模腔的模具中的高压、热注射模塑操作。部件在模腔内冷却，然后从模具中推出。所有过程在大约170℃-180℃下进行。然后在烧结前对生坯件施以在异丙醇中的脱脂。脱脂从该部件中清除一部分有机粘合剂并留下刚好足以保持内聚(或换言之，保持生坯件的模制形状)的粘合剂。通常通过加热将该生坯件浸在其中的溶剂而从生坯件中除去粘合剂。在该操作过程中，必须溶解至少40％的粘合剂化合物。对于本发明的粘合剂，通常将生坯件浸在异丙醇溶剂中并加热到大约70℃的温度。在该温度下，蜡混合物或蜡和油混合物热分解，而表面活性剂和异丙醇可溶聚合物化学溶解。一旦溶剂脱脂操作完成，该部件多孔。然后将该部件置于高温炉中以首先清除剩余粘合剂(热脱脂，通常在小于400℃的温度下)，在溶剂脱脂过程中留在部件中的孔隙促进这一操作，其次在高温下烧结该部件。
根据无机粉末的性质，由具有下表I中所示的组成的本发明的各种粘合剂根据上述方法制造部件：
表I
Figure BDA0002042975300000071
这些组分可购得。乙烯-丙烯共聚物(无规聚丙烯共聚物)是Total Refining&Chemicals分销的PPR 10232。马来酸酐接枝的聚丙烯是DuPontTM分销的
Figure BDA0002042975300000072
P353。乙酸丁酸纤维素是EastmanTM分销的CAB-551-0.01。
根据上述实施例1用Saint-Gobain Zir Black黑色氧化锆ZrO2粉末作为有机粉末制造组合物。用具有1mm直径和20mm长度模头的Instron Ceast SR20毛细管流变仪测量这种组合物的粘度。
作为比较，测量使用相同Saint-Gobain Zir Black黑色无机氧化锆ZrO2粉末的专利申请No.WO 2014/191304的实施例1中公开的原料组合物的粘度。
结果列在下表II中：
表II
Figure BDA0002042975300000081
根据本发明的注射模塑组合物在同等剪切速率下具有比已知原料低的粘度。
此外，在异丙醇溶剂中的脱脂过程中的粘合剂清除得以改进：在该溶剂中清除专利申请WO2014/191304中描述的粘合剂的大约45％，而本发明的粘合剂被清除了至少50％，尤其是乙酸丁酸纤维素。在金属粉末的情况下，清除百分比可高达65％。
所得模制和烧结部件具有改进的表面外观，没有可见裂缝或焊接线。

Claims (16)

1.用于注射模塑组合物的粘合剂，其包括，作为组分：
-40至55体积％的聚合物基料，
-35至45体积％的蜡混合物或蜡和棕榈油的混合物，
-和至少5体积％的至少一种表面活性剂，
其中所述聚合物基料由以下各项形成：
乙烯与甲基丙烯酸或丙烯酸的共聚物，
乙烯与丙烯的共聚物和/或马来酸酐接枝的聚丙烯，和
可溶于选自异丙醇、丙醇、松节油及其混合物的溶剂并选自乙酸丁酸纤维素、聚乙烯醇缩丁醛和共聚酰胺的聚合物，
粘合剂组分各自的量使得它们的总和等于100体积％的粘合剂。
2.根据权利要求1的粘合剂，其特征在于所述聚合物基料包括2至7体积％的乙烯与甲基丙烯酸或丙烯酸的共聚物、0至40体积％的乙烯与丙烯的共聚物、0至35体积％的马来酸酐接枝的聚丙烯，其中乙烯与丙烯的共聚物和马来酸酐接枝的聚丙烯的量在30至40体积％之间，和6至15体积％的可溶于选自异丙醇、丙醇、松节油及其混合物的溶剂的聚合物，至100体积％的粘合剂，粘合剂组分各自的量使得它们的总和等于100体积％的粘合剂。
3.根据权利要求1的粘合剂，其特征在于所述聚合物基料包括乙烯与丙烯的共聚物和马来酸酐接枝的聚丙烯的混合物。
4.根据权利要求3的粘合剂，其特征在于所述聚合物基料包括2至7体积％的乙烯与甲基丙烯酸或丙烯酸的共聚物、25至30体积％的乙烯与丙烯的共聚物、5至10体积％的马来酸酐接枝的聚丙烯和6至15体积％的可溶于选自异丙醇、丙醇、松节油及其混合物的溶剂的聚合物，至100体积％的粘合剂。
5.根据权利要求1的粘合剂，其特征在于所述乙烯与丙烯的共聚物是熔点在140℃至150℃之间的无规统计乙烯-丙烯共聚物。
6.根据权利要求1的粘合剂，其特征在于所述乙烯与甲基丙烯酸或丙烯酸的共聚物含有3至10重量％的甲基丙烯酸或丙烯酸系共聚单体。
7.根据权利要求1的粘合剂，其特征在于所述马来酸酐接枝的聚丙烯具有1％至2％接枝率和100℃至140℃的熔点。
8.根据权利要求1的粘合剂，其特征在于所述可溶于选自异丙醇、丙醇、松节油及其混合物的溶剂的聚合物是具有相对于聚合物重量计37重量％至53重量％的丁酰基含量、2重量％至13重量％的乙酰基含量、125℃至165℃的熔点和16000至40000的分子量的乙酸丁酸纤维素。
9.根据权利要求1的粘合剂，其特征在于所述蜡是巴西棕榈蜡、石蜡或其混合物。
10.根据权利要求1的粘合剂，其特征在于所述蜡和棕榈油的混合物中的蜡是巴西棕榈蜡。
11.根据权利要求1的粘合剂，其特征在于所述表面活性剂是N,N'-亚乙基双(硬脂酰胺)，或硬脂酸和棕榈酸的混合物，或这些成分的混合物。
12.根据权利要求1的粘合剂，其特征在于所述表面活性剂可溶于选自异丙醇、丙醇、松节油及其混合物的溶剂。
13.意图用于制造成型金属或陶瓷部件的注射模塑组合物(原料)，其包括76至96重量％的无机粉末和4至24重量％的用于注射模塑组合物的粘合剂，所述粘合剂包括，作为组分：
-40至55体积％的聚合物基料，
-35至45体积％的蜡混合物或蜡和棕榈油的混合物，
-和至少5体积％的至少一种表面活性剂，
其中所述聚合物基料由以下各项形成：
乙烯与甲基丙烯酸或丙烯酸的共聚物，
乙烯与丙烯的共聚物和/或马来酸酐接枝的聚丙烯，和
可溶于选自异丙醇、丙醇、松节油及其混合物的溶剂并选自乙酸丁酸纤维素、聚乙烯醇缩丁醛和共聚酰胺的聚合物，
粘合剂组分各自的量使得它们的总和等于100体积％的粘合剂。
14.根据权利要求13的模塑组合物，其中所述无机粉末选自氧化物粉末、氮化物粉末、碳化物粉末、金属粉末或其混合物。
15.根据权利要求14的模塑组合物，其中所述无机粉末选自氧化铝粉末、氧化锆粉末、碳化铬粉末、碳化钛粉末或碳化钨粉末、金属钨或氮化硅粉末、不锈钢粉末、金属钛粉末或所述粉末的混合物。
16.根据权利要求15的模塑组合物，其含有按重量％计：
·76至88％的氧化铝和12至24％的粘合剂，
·76至88％的氧化铝和0.1至0.6％的氧化镁和12至24％的粘合剂，
·58至86.5％的氧化锆和3.9至4.6％的氧化钇和0.18至18.5％的氧化铝和9至22％的粘合剂，
·61.5至84％的氧化锆和3.9至4.6％的氧化钇和0.2至9％的氧化铝和2至5.5％的选自氧化铁、氧化钴、氧化铬、氧化钛、氧化锰、氧化锌或所述氧化物的混合物的无机颜料和9至22％的粘合剂，
·88至91％的铬或钛碳化物，和9至12％的粘合剂，
·93至96％的碳化钨或金属钨和4至7％的粘合剂，或
·78至85％的氮化硅，和15至22％的粘合剂。
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EP3563950B1 (fr) 2023-11-01
PT115469A (pt) 2019-06-03
PT115469B (pt) 2021-06-18
US11718736B2 (en) 2023-08-08
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JP2019194009A (ja) 2019-11-07
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