CN1743164A - 液晶聚酯树脂组合物部件接合方法和由其构成的接合制品 - Google Patents

液晶聚酯树脂组合物部件接合方法和由其构成的接合制品 Download PDF

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Publication number
CN1743164A
CN1743164A CNA2005100687895A CN200510068789A CN1743164A CN 1743164 A CN1743164 A CN 1743164A CN A2005100687895 A CNA2005100687895 A CN A2005100687895A CN 200510068789 A CN200510068789 A CN 200510068789A CN 1743164 A CN1743164 A CN 1743164A
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polyester resin
liquid
crystal polyester
welding
parts
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CN1743164B (zh
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北山雅也
齐藤尚示
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Ueno Seiyaku Oyo Kenkyujo KK
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Ueno Seiyaku Oyo Kenkyujo KK
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
    • C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
    • C08G63/60—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from the reaction of a mixture of hydroxy carboxylic acids, polycarboxylic acids and polyhydroxy compounds
    • C08G63/605—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from the reaction of a mixture of hydroxy carboxylic acids, polycarboxylic acids and polyhydroxy compounds the hydroxy and carboxylic groups being bound to aromatic rings
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/01—General aspects dealing with the joint area or with the area to be joined
    • B29C66/05—Particular design of joint configurations
    • B29C66/10—Particular design of joint configurations particular design of the joint cross-sections
    • B29C66/12—Joint cross-sections combining only two joint-segments; Tongue and groove joints; Tenon and mortise joints; Stepped joint cross-sections
    • B29C66/126—Tenon and mortise joints
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/50—General aspects of joining tubular articles; General aspects of joining long products, i.e. bars or profiled elements; General aspects of joining single elements to tubular articles, hollow articles or bars; General aspects of joining several hollow-preforms to form hollow or tubular articles
    • B29C66/51—Joining tubular articles, profiled elements or bars; Joining single elements to tubular articles, hollow articles or bars; Joining several hollow-preforms to form hollow or tubular articles
    • B29C66/54—Joining several hollow-preforms, e.g. half-shells, to form hollow articles, e.g. for making balls, containers; Joining several hollow-preforms, e.g. half-cylinders, to form tubular articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C66/731—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the intensive physical properties of the material of the parts to be joined
    • B29C66/7311—Thermal properties
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    • B29C66/737—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the state of the material of the parts to be joined
    • B29C66/7377—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the state of the material of the parts to be joined amorphous, semi-crystalline or crystalline
    • B29C66/73775—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the state of the material of the parts to be joined amorphous, semi-crystalline or crystalline the to-be-joined area of at least one of the parts to be joined being crystalline
    • B29C66/73776—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the state of the material of the parts to be joined amorphous, semi-crystalline or crystalline the to-be-joined area of at least one of the parts to be joined being crystalline the to-be-joined areas of both parts to be joined being crystalline
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/73—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset
    • B29C66/739—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of the parts to be joined being a thermoplastic or a thermoset
    • B29C66/7392—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of at least one of the parts being a thermoplastic
    • B29C66/73921—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of at least one of the parts being a thermoplastic characterised by the materials of both parts being thermoplastics
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/73—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset
    • B29C66/739—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of the parts to be joined being a thermoplastic or a thermoset
    • B29C66/7394—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of at least one of the parts being a thermoset
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29K2509/00—Use of inorganic materials not provided for in groups B29K2503/00 - B29K2507/00, as filler
    • B29K2509/10—Mica

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)
  • Polyesters Or Polycarbonates (AREA)
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Abstract

本发明提供接合液晶聚酯树脂组合物部件的方法，特征在于由差示扫描量热计测量的液晶聚酯树脂的熔点是190－250℃和各个部件利用焊接来接合。通过使用本发明的方法，以精确度获得具有足够的接合强度的接合制品。

Description

液晶聚酯树脂组合物部件接合方法和 由其构成的接合制品
技术领域
本发明涉及接合液晶聚酯树脂组合物部件的方法和由接合方法获得的由液晶聚酯树脂组合物构成的接合制品。
背景技术
热致液晶聚酯树脂(以下称作“液晶聚酯树脂”或“LCP”)显示出良好的模塑流动性和优异的热稳定性，因此，广泛地用于制造模制品，尤其，具有薄而小的部件如小螺距接头的电子元件。LCP还具有良好的机械性能，其中包括良好的刚性和优异的耐化学品性，和气体阻隔性能和显示出高的尺寸精确度。由于这些性能，LCP不仅用于制造模制品而且用于制造包括纤维和膜在内的各种产品。
最近，由LCP构成的模制品、纤维或膜的二次制造已在现有技术中引起关注。在通常已知的二次制造方法之中，接合方法如粘结和焊接已经得到了人们的大量关注。尤其，广泛地用于制造多用途的塑料的方法，即利用摩擦热焊接树脂部件的方法，已经预期作为制造液晶聚酯树脂部件的备选方法。
然而，广泛分布的普通液晶聚酯树脂具有高达280-400℃的极高熔点，因此，LCP不能由普通的焊接方法来焊接，或即使能够焊接，所获得的焊接产品的接合部分因为缺乏强度而使得无法实际应用。已经建议了焊接液晶聚酯树脂部件的一些改进方法。例如，JP A H03-184830公开了具有高熔点的树脂如液晶聚酯树脂的超声波焊接的改进方法，它包括预先加热树脂到某个温度范围，然后焊接该树脂。这一方法能够确保在超声波焊接技术中的接合。
具体地说，在该方法中，需要接合的树脂部件如具有高于250℃的熔点的LCP利用外部加热设备如空气烘箱或通过加热支持体(它能够利用加热介质或加热设备来加热)来进行预热，然后进行超声波焊接。该方法能够确保焊接和减少被焊接的模制品的变形或破坏。
然而，从成本和效率考虑该方法是不令人满意的，归因于需要外部加热设备或内部支持体加热设备的附加预热步骤。另外，由于高预热温度所引起的焊接制品的软化或变形，该方法是不实用的。
本发明内容
本发明的目的是提供接合液晶聚酯树脂组合物部件的方法，它确保了接合的精确度和能够提供具有优异的接合强度的接合制品。本发明的另一个目的是提供由LCP构成的接合制品，其中由LCP组成的两个或多个部件由本发明的方法强力地接合。
本发明提供接合液晶聚酯树脂组合物部件的方法，特征在于包含于组合物中的液晶聚酯树脂的熔点(由差示扫描量热计测量)是190-250℃和部件利用焊接方式来接合。
本发明还提供可由该接合方法获得的液晶聚酯树脂组合物的接合制品。
在这里使用的“由液晶聚酯树脂组合物构成的接合制品”是指由液晶聚酯树脂组合物构成的并具有由本发明的方法形成的接合部分的产品。
在本发明中使用的“液晶聚酯树脂组合物”可包括0-100重量份/每100重量份的液晶聚酯树脂的填料和/或增强材料。
根据本发明的方法，能够获得具有良好的精确度和高的接合强度的由液晶聚酯树脂组合物构成的接合制品。
附图说明
图1描绘了在实施例中使用的斜面接合(scarf joint)。
图2描绘了在实施例中使用的剪切接合(shear joint)。
包含在本发明中所用的液晶聚酯树脂组合物中的液晶聚酯树脂没有具体地限制，并可以是具有190-250℃的熔点(由差示扫描量热计测量)，显示出各向异性熔体相和由本领域中的技术人员称作热致型液晶聚酯树脂的任何聚酯树脂。
各向异性熔体相能够利用使用正交光偏振器的普通偏振光***来证实。更详细地说，在氮气氛中在Leitz热台上的样品可以用Leitz偏光显微镜观察。
用于本发明中的由差示扫描量热计测定的熔点等于或高于190℃和低于250℃的液晶聚酯树脂可以是半芳族液晶聚酯树脂或全芳族液晶聚酯树脂。在本说明书和权利要求中，“半芳族液晶聚酯树脂”表示脂肪族-芳族LCP，它在分子链中具有脂肪族结构部分。全芳族液晶聚酯树脂表示每一个重复单体单元为聚合物骨架贡献至少一个芳族核的LCP。
在这些液晶聚酯树脂之中，全芳族液晶聚酯树脂是优选的，因为它们的阻燃性和良好机械性能。
用于制备在本发明中使用的液晶聚酯树脂的重复单元的例子是芳族氧基羰基重复单元，芳族二-羰基重复单元，芳族二氧基重复单元，芳族氧基二-羰基重复单元和脂肪族二氧基重复单元。
由上述重复单元组成的液晶聚酯树脂既包括可得到各向异性熔体相的那些和又包括不得到各向异性熔体相的那些，这取决于结构组分或树脂以及它们的比率，和序列分布。用于本发明中的液晶聚酯树脂限于显示出各向异性熔体相的那些。
提供芳族氧基羰基重复单元的单体的例子是对-羟基苯甲酸，间-羟基苯甲酸，邻-羟基苯甲酸，6-羟基-2-萘甲酸，5-羟基-2-萘甲酸，3-羟基-2-萘甲酸，4’-羟苯基-4-苯甲酸，3’-羟苯基-4-苯甲酸，4’-羟苯基-3-苯甲酸，和它们的烷基-，烷氧基-或卤素-取代的衍生物以及它们的酯形成用衍生物如酰基衍生物，酯衍生物和酰卤。在以上之中，就控制所制备液晶聚酯树脂的性能和熔点而言，对羟基苯甲酸和6-羟基-2-萘甲酸是优选的。
提供芳族二-羰基重复单元的单体的例子是芳族二羧酸类，如对苯二甲酸，间苯二酸，2，6-萘二甲酸，1，6-萘二甲酸，2，7-萘二甲酸，1，4-萘二甲酸，4，4’-二羧基联苯，双(4-羧基苯基)醚，双(3-羧基苯基)醚，和它们的烷基-，烷氧基或卤素-取代的衍生物以及它们的酯形成用衍生物如酯衍生物，酰卤。在以上之中，就控制所制备液晶聚酯树脂的机械性能，耐热性，熔点和模塑加工性能而言，对苯二甲酸和2，6-萘二甲酸是优选的。
提供芳族二氧基重复单元的单体的例子是芳族二醇如氢醌，间苯二酚，2，6-二羟基萘，2，7-二羟基萘，1，6-二羟基萘，1，4-二羟基萘，4，4’-二羟基联苯，3，3’-二羟基联苯，3，4’-二羟基联苯，4，4’-二羟基二苯基醚，和它们的烷基-，烷氧基-或卤素-取代的衍生物以及它们的酯形成用衍生物如酰基衍生物。在以上之中，对于在聚合过程中的良好反应活性和所制备的液晶聚酯树脂的良好性能而言，氢醌和4，4’-二羟基联苯是优选的。
提供芳族氧基二-羰基重复单元的单体的例子是羟基芳族二羧酸如3-羟基-2，7-萘二甲酸，4-羟基-间苯二酸，5-羟基-间苯二酸，和它们的烷基-，烷氧基-或卤素-取代的衍生物以及它们的酯形成用衍生物如酰基衍生物，酯衍生物和其酰卤。
提供脂肪族二氧基重复单元的单体的例子是脂肪族二醇如乙二醇，1，4-丁二醇，1，6-己二醇，和它们的酰基衍生物。另外，具有脂肪族二氧基重复单元的液晶聚酯树脂能够通过具有脂肪族二氧基重复单元的聚酯如聚对苯二甲酸乙二醇酯或聚对苯二甲酸丁二醇酯与以上芳族氧基羧酸，芳族二羧酸，芳族二醇或它们的酰基衍生物，酯衍生物或其酰卤反应来获得。
在以上之中，考虑到它们的低熔点和良好机械性能，用于本发明中的优选液晶聚酯树脂是主要由下列结构式(I)，(II)，(III)和(IV)表示的重复单元组成的那些：
Figure A20051006878900072
Figure A20051006878900073
Figure A20051006878900074
其中：
Ar1和Ar2各表示至少一个二价芳族基；和
p，q，r和s表示在液晶聚酯树脂中重复单元的相对摩尔比例(mol％)和满足下面公式：
0.4≤p/q≤2.0
2mol％≤r≤15mol％
2mol％≤s≤15mol％。
在以上之中，下面给出了重复单元的优选的组合。
Figure A20051006878900081
在以上之中，尤其优选的重复单元的组合是如下：
Figure A20051006878900082
其中：在单元之下的值表示在液晶聚酯树脂中各重复单元的mol％量。
用于本发明中的液晶聚酯树脂可以具有酰胺键或硫酯键，只要此类键不损害本发明的目的。提供酰胺键或硫酯键的单体的例子是芳族羟氨，芳族二胺，芳族氨基羧酸，巯基芳族羧酸，芳族二硫醇和巯基芳族酚。以提供芳族氧基羰基重复单元，芳族二-羰基重复单元，芳族二氧基重复单元，芳族氧基二-羰基重复单元和脂肪族二氧基重复单元的单体的总量为基础，这些附加单体的比例优选是不高于10mol％。
另外，用于本发明的液晶聚酯树脂可以是通过将两种或多种的由差示扫描量热计测定的熔点在190-250℃范围内的液晶聚酯树脂加以共混所获得的那些。
制备用于本发明的液晶聚酯树脂的方法没有限制，并且能够使用本领域中技术人员已知的任何方法。例如，用于制备聚酯以便在上述单体组分之间形成酯键的普通聚合方法如熔融酸解和淤浆聚合方法都可以使用。
熔融酸解方法优选用于制备在本发明中使用的液晶聚酯树脂。在这一方法中，将单体加热而获得熔融的溶液，然后让溶液反应而得到熔融聚合物。这一的最后步骤可以在真空下进行以促进挥发性副产物如乙酸或水的除去。
该淤浆聚合方法体现特征在于：单体在热交换流体中反应得到了在热交换液体介质中的悬浮液形式的固态聚合物。
在熔融酸解方法或淤浆聚合方法之中的任何一种方法中，聚合用单体组分可以在呈现变性形式，即作为低级酰基酯，它能够通过在室温下将羟基加以酯化来获得。低级酰基优选具有2-5个，更优选2-3个碳原子。乙酸酯最优选用于该反应。
此类单体的低级酰基酯可以是通过将各单体独立地酰化所预先制备的那些或可以是在制备液晶聚酯过程中将酰化剂如乙酸酐添加到单体中而在反应体系中产生的那些。
在熔融酸解方法或淤浆聚合方法之中的任何一种方法中，如果需要的话，催化剂可以用于反应中。
催化剂的例子包括有机锡化合物，如二烷基锡氧化物(例如***)和二芳基锡氧化物；有机钛化合物如二氧化钛，三氧化锑，烷氧基钛硅酸盐和钛醇盐；羧酸的碱金属或碱土金属盐如乙酸钾；无机酸的盐(例如K2SO4)和气体酸催化剂如路易斯酸(例如BF3)和卤化氢(例如HCl)。
当使用催化剂时，以总单体为基础计算，被添加到反应中的催化剂的量优选是10-1000ppm，和更优选20-200ppm。
根据本发明，由差示扫描量热计(DSC)通过下述方法测定的液晶聚酯树脂的熔点等于或高于190℃和低于250℃，优选200-245℃和尤其210-240℃。
测定LCP的熔点的详细方法是如下：
可以使用差示扫描量热计Exstar 6000(Seiko InstrumentsInc.，Chiba，Japan)或相同类型的DSC设备。被考察的LCP样品以20℃/分钟的速率加热和记录吸热峰(Tm1)。其后，LCP样品在比Tm1高20-50℃的温度下保持10分钟。然后以20℃/分钟的速率被冷却至室温，然后以相同的速率再次加热。在最终步骤中测定的吸热峰被记录为熔点。
优选，用于本发明中的液晶聚酯树脂要求它的log粘度在五氟苯酚中测量。在60℃下以在五氟苯酚中0.1g/dl的浓度测量的聚合物的log粘度优选是0.3dl/g或0.3dl/g以上，更优选0.5-10dl/g，最优选1-8dl/g。
用毛细管流变仪测量的用于本发明中的液晶聚酯树脂的熔体粘度可优选是1-1000Pa.s，更优选5-300Pa.s。
该液晶聚酯树脂可以从聚合反应容器中以熔融相获取，并加工得到粒料，碎屑料或粉末料。
用于本发明中的液晶聚酯树脂组合物可以是通过将一种或多种纤维状，层状或微粒状填料和/或增强材料与液晶聚酯树脂掺混所获得的那些。
纤维状填料和/或增强材料的例子可以包括玻璃纤维，硅石-氧化铝纤维，氧化铝纤维，碳纤维和聚芳酰胺纤维。在它们之中，玻璃纤维是优选使用的，因为它的物理性能和成本的良好平衡。
层状或微粒状填料和/或增强材料的例子可以包括滑石，云母，石墨，硅灰石，碳酸钙，白云石，粘土，玻璃屑，玻璃珠，硫酸钡和二氧化钛。
该填料和/或增强材料是以0-100重量份，优选10-90重量份/每100重量份的液晶聚酯树脂的用量被添加到用于本发明中的液晶聚酯树脂组合物中。如果填料和/或增强材料的量大于100重量份，则所形成的液晶聚酯树脂组合物的模塑性能倾向于下降或模塑设备的机筒或模头的消耗会增加，此外，由于在接合的制品中低树脂含量，使得LCP的接合处的强度倾向于下降。
如果需要，根据本发明的液晶聚酯树脂组合物可以进一步与通常用于树脂组合物的一种或多种添加剂进行掺混。例如，模塑用润滑剂如高级脂肪酸，高级脂肪族酯，高级脂肪族酰胺，高级脂肪酸金属盐，聚硅氧烷和碳氟树脂；着色剂如染料和颜料；抗氧化剂；热稳定剂；UV吸收剂；抗静电剂；和表面活性剂可以掺混进去。模塑用润滑剂如高级脂肪酸，高级脂肪族酯，高级脂肪酸金属盐或碳氟型表面活性剂可以在粒料进行模塑加工之前被添加到液晶聚酯树脂或液晶聚酯树脂组合物的粒料中，这样添加剂粘附于粒料的外表面。
优选，从模塑性和物理性能考虑，用于本发明的液晶聚酯树脂组合物的树脂组分主要由液晶聚酯树脂组成。然而，本发明的液晶聚酯树脂组合物可以包括一种或多种附加树脂组分，它们具有由差示扫描量热计测定的190-250℃的熔点，只要这些附加树脂组分不损害本发明的目的。附加树脂组分的例子包括热塑性树脂如聚酰胺，聚酯，聚苯硫醚，聚醚酮，聚碳酸酯，聚苯醚和它们的变性衍生物，聚砜，聚醚砜和聚醚酰亚胺和热固性树脂如酚醛树脂，环氧树脂和聚酰亚胺树脂。附加树脂组分的量没有限制，并根据预定的性能来确定。典型地，此类附加树脂是以0-150重量份，优选40-100重量份/每100重量份的液晶聚酯树脂的用量被添加到液晶聚酯树脂组合物中。
用于本发明的液晶聚酯树脂组合物可以通过将填料、增强材料和其它树脂组分添加到液晶聚酯树脂中和然后使用捏和机器如班伯里密炼机，捏合机，单螺杆挤出机，双螺杆挤压机等熔融捏合该混合物来获得。
该液晶聚酯树脂组合物可以按照普通的方式加工得到需要接合在一起的部件，如模制品，膜，片，粘合型纺织品等等。例如，注塑或挤出技术优选用于获得需要接合的部件。
根据本发明，由特定的液晶聚酯树脂组合物组成的部件被焊接。适宜用于本发明的焊接方法的例子是超声波焊接，高频焊接，电磁感应焊接，脉冲焊接，振动焊接和旋转焊接。
下面简要描述这些接合方法(焊接方法)。
<超声波焊接>
在本方法中，超声波电能转化成机械振动能，后者在需要焊接的树脂部件的接合面感应摩擦热，使得它们能够焊接在一起。
<高频焊接>
在本方法中，利用高频辐射在需要焊接的部件内部产生介质热，使它们焊接在一起。
<电磁感应焊接>
在本方法中，放置在待焊接的部件的接合部分上的金属或磁性材料有选择地加热，使得各部件间接加热和使它们焊接在一起。
<脉冲焊接>
在本方法中，各部件利用压板加压，然后装配在压板顶部的镍铬丝带瞬间受热来软化或熔融该部件以使它们焊接在一起。
<振动焊接>
在这一方法中，需要焊接的两个部件处于压力下，它们中的一个沿水平方向振动在焊缝表面上感应摩擦热，以使各部件焊接在一起。
<旋转焊接>
在本方法中，圆形模塑部件处于压力下，该制品在高速下旋转以感应摩擦热，然后各部件被焊接。
从大型或复杂形状的制品的焊接性考虑，在上述接合/焊接方法之中，超声波焊接、振动焊接或旋转焊接对于本发明是尤其优选的。
对于使用超声波焊接，振动焊接或旋转焊接的情况，各部件优选是以提供斜面接合或剪切接合的方式来接合。
斜面接合(scarf joint)是通过将具有搭接在一起的变截面、倾斜面或倒角型末端的两个构件相接合来形成的。它在两个变截面之间形成平面型接触，它们的表面均匀地被加热和导致足够的焊接面积。因此，斜面接合能够提供很高的接合强度。
剪切接合是通过焊接具有凸出部的第一部件和具有接受凸出部的凹陷的第二部件来形成的，其中振动施加于第一部件的边缘和第二部件的渐变部分。在剪切接合中，接合部分以高的热产生效率来加热，因此能够获得强焊接的制品。另外，因为各部件的接触方向和振动方向几乎相当，几乎不在焊缝表面上形成气泡并能够获得具有水密性和气密性的接合制品。
在本发明的液晶聚酯树脂组合物部件的接合方法中，某些部件利用焊接来接合。也就是说，需要焊接的部件是由含有液晶聚酯树脂的液晶聚酯树脂组合物组成，由差示扫描量热计测定的该树脂的熔点是高于或等于190℃和低于250℃。根据本发明的方法，各个部件的接合用表面容易地熔融和因此，能够制造出具有足够的接合强度的液晶聚酯树脂组合物的接合制品。
另外，本发明的接合方法有利于模制品的二次制造，如具有薄壁的或属于精细部件的那些模制品，它们能够通过使用具有优异的模塑性的液晶聚酯树脂来获得。例如，利用本发明有可能通过焊接具有薄壁的小型部件来制造用于空调器等的室内设备的具有薄壁的小型交叉流风扇。
另外，根据本发明，容易密封膜或粘合型纺织品，因此有可能生产具有良好气密性或耐化学性的袋或类似物。
具体实施方式
本发明进一步参考下列实施例来描述。
实施例
在实施例中使用下列缩写。
<组成液晶聚酯树脂的单体>
BON6：6-羟基-2-萘甲酸
POB：对羟基苯甲酸
HQ：氢醌
BP：4，4’-二羟基联苯
TPA：对苯二甲酸
IPA：间苯二酸
合成实施例1
LCP-I的合成
将BON6、POR、HQ和TPA以表1中所示的比率加入到装有带扭矩测量仪的搅拌装置和冷凝器的反应容器中，以使总单体量是5mol。然后将乙酸钾0.05g(相对于单体总量而言的67mol ppm)和相对于单体羟基的总量(mol)而言1.025倍mol量的乙酸酐加入到容器中。混合物在下面条件下聚合。
表1
合成实施例1：单体比
    BON6     POB     HQ     TPA
    G     386     297     44     67
    mol％     41     43     8     8
在氮气氛中，经过1小时将混合物从室温加热到150℃并在150℃下保持30分钟，然后快速地加热到210℃而同时馏出副产物乙酸并在这一温度下保持30分钟。然后混合物经过3小时被加热至335℃和压力经过30分钟降至20mmHg。当扭矩变成预定的水平时，停止聚合反应。将所形成的树脂从容器中排出并由破碎机破碎而得到LCP的粒料。结果，馏出了大约理论量的乙酸。
由DSC测定的液晶聚酯树脂的熔点是218℃。
合成实施例2
LCP-II的合成
将POB和BON6以表2中所示的比率加入到装有带扭矩测量仪的搅拌装置和冷凝器的反应容器中，以使总单体量是5mol。然后将乙酸钾0.05g(相对于单体总量而言的67mol ppm)和相对于单体羟基的总量(mol)而言1.025倍mol量的乙酸酐加入到容器中并由下列条件进行聚合反应。
表2
合成实施例2：单体比
  POB   BON6
  g   504.2   254.0
  mol％   73   27
在氮气氛中，经过1小时将混合物从室温加热到150℃并在150℃下保持30分钟，然后快速地加热到210℃而同时馏出副产物乙酸并在这一温度下保持30分钟。然后混合物经过3小时被加热至325℃和压力经过30分钟降至20mmHg。当扭矩变成预定的水平时，停止聚合反应。将所形成的树脂从容器中排出并由破碎机破碎而得到LCP的粒料。结果，馏出了大约理论量的乙酸。
由DSC测定的液晶聚酯树脂的熔点是280℃。
合成实施例3
LCP-III的合成
将POB、BP、TPA和IPA以表3中所示的比率加入到装有带扭矩测量仪的搅拌装置和冷凝器的反应容器中，以使总单体量是5mol。然后将乙酸钾0.05g(相对于单体总量而言的67mol ppm)和相对于单体羟基的总量(mol)而言1.025倍mol量的乙酸酐加入到容器中并由下列条件进行聚合反应。
表3
合成实施例3：单体比
  POB   BP   TPA   IPA
  g   414.4   186.2   83.1   83.1
  mol％   60   20   10   10
在氮气氛中，经过1小时将混合物从室温加热到150℃并在150℃下保持30分钟，然后快速地加热到210℃而同时馏出副产物乙酸并在这一温度下保持30分钟。然后混合物经过3小时被加热至350℃和压力经过30分钟降至20mmHg。当扭矩变成预定的水平时，停止聚合反应。将所形成的树脂从容器中排出并由破碎机破碎而得到LCP的粒料。结果，馏出了大约理论量的乙酸。
由DSC测定的液晶聚酯树脂的熔点是330℃。
实施例1和2
将按表4中所示的用量的玻璃纤维(FT 562，ASAHI FIBER GLASSCo.，Tokyo，Japan)(B)或碳纤维(HTA-C6-S，TOHO TENAX Co. Tokyo，Japan)(C)与100重量份的液晶聚酯树脂，LCP-I(A)用Henschel混合器进行混合，然后由双螺杆挤出机(TEX 30α，The Japan Steel works，LTD.，Tokyo，Japan)以235℃的机筒温度挤出，得到液晶聚酯树脂组合物的粒料。所形成的粒料在130℃下干燥4小时并通过注塑机(α-100iA，FANUC LTD，Yamanashi，Japan)以240℃的机筒温度和70℃的模头温度进行模塑，得到具有适合于图1中所示的斜面接合的形状的和适合于图2中所示的剪切接合的形状的那些部件。
所形成的模塑部件利用超声波焊接机(BRANSON 950M，EmersonJapan，Ltd.)在下列条件下焊接，得到接合的制品。
接合的制品的接合强度通过使用Instron Corporation # 5567在与接合面垂直的方向上在5mm/sec的拉伸速率下作为断裂力来评价的。结果示于表4中。
<超声波焊接条件>
振动：20KHz
喇叭：圆锥形喇叭，TIN，3/4英寸直径
焊接时间：80毫秒
持续时间：0.5秒
对比实施例1和2
按照与实施例1同样的程序制备接合的制品，只是使用LCP-II，代替LCP-I并使用300℃的机筒温度和70℃的模头温度的注塑条件。接合强度的评价是由与实施例1相同的程序进行的。结果示于表4中。
对比实施例3和4
按照与实施例1同样的程序制备接合的制品，只是使用LCP-III，代替LCP-I并使用350℃的机筒温度和70℃的模头温度的注塑条件。接合强度的评价是由与实施例1相同的程序进行的。结果示于表4中。
表4
A：液晶聚酯树脂
B：玻璃纤维(ASAHI FIBER GLASS Co.，FT 562)
C：碳纤维(TOHO TENAX Co，HTA-C6-S)
D：液晶聚酯树脂的熔点
E：斜面接合的接合强度
F：剪切接合的接合强度
  A(树脂/重量份) B(重量份) C(重量份)   D(℃)   E(N)   F(N)
  实施例1   LCP-I/100 42.8 0   218   330   355
  实施例2   LCP-I/100 0 42.8   218   340   370
  对比例1   LCP-II/100 42.8 0   280   290   245
  对比例2   LCP-II/100 0 42.8   280   295   270
  对比例3   LCP-III/100 42.8 0   330   205   195
  对比例4   LCP-III/100 0 42.8   330   215   200

Claims (10)

1.接合液晶聚酯树脂组合物部件的方法，特征在于由差示扫描量热计测量的液晶聚酯树脂的熔点是190-250℃和这些部件利用焊接来接合。
2.根据权利要求1的方法，其中树脂主要由下面结构式(I)，(II)，(III)和(IV)表示的重复单元组成：
Figure A2005100687890002C1
其中：
Ar1和Ar2各自表示至少一个二价芳族基团；和
p，q，r和s表示在液晶聚酯树脂中重复单元的相对摩尔比例(mol％)和满足下面公式：
                 0.4≤p/q≤2.0
                 2mol％≤r≤15mol％
                 2mol％≤s≤15mol％。
3.根据权利要求1或2的方法，其中所述液晶聚酯树脂由下列重复单元组成：
其中：
在重复单元之下的值表示在液晶聚酯树脂中各单元的mol％。
4.根据权利要求1-3中任何一项的方法，其中所述焊接是选自超声波焊接，振动焊接，高频焊接，电磁感应焊接，脉冲焊和旋转焊接。
5.根据权利要求1-3中任何一项的方法，其中所述焊接是超声波焊接，振动焊接或旋转焊接，和所述液晶聚酯树脂组合物部件被焊接形成了选自斜面接合和剪切接合中的接合。
6.根据权利要求1-5中任何一项的方法，其中液晶聚酯树脂组合物包括0-100重量份/每100重量份的液晶聚酯树脂的填料和/或增强材料。
7.根据权利要求6的方法，其中填料和/或增强材料是选自玻璃纤维，硅石-氧化铝纤维，氧化铝纤维，碳纤维，聚芳族酰胺纤维，滑石，云母，石墨，硅灰石，碳酸钙，白云石，粘土，玻璃屑，玻璃珠，硫酸钡和二氧化钛中的至少一种。
8.根据权利要求7的方法，其中所述填料和/或增强材料是玻璃纤维。
9.由液晶聚酯树脂组合物得到的接合制品，它可由根据权利要求1-8中任何一项的方法获得。
10.根据权利要求9的接合制品，其中所述接合的制品是由部件组成，该部件选自模制品，膜，片和粘合型纺织品。
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