TWI820295B - 熱膨脹性微膠囊及發泡成形用組成物 - Google Patents
熱膨脹性微膠囊及發泡成形用組成物 Download PDFInfo
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- TWI820295B TWI820295B TW109102795A TW109102795A TWI820295B TW I820295 B TWI820295 B TW I820295B TW 109102795 A TW109102795 A TW 109102795A TW 109102795 A TW109102795 A TW 109102795A TW I820295 B TWI820295 B TW I820295B
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Classifications
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/102—Azo-compounds
- C08J9/103—Azodicarbonamide
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/32—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof from compositions containing microballoons, e.g. syntactic foams
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- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
- B01J13/18—In situ polymerisation with all reactants being present in the same phase
- B01J13/185—In situ polymerisation with all reactants being present in the same phase in an organic phase
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08F220/42—Nitriles
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08F220/48—Acrylonitrile with nitrogen-containing monomers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J9/141—Hydrocarbons
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- C08J9/20—Making expandable particles by suspension polymerisation in the presence of the blowing agent
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
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- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/22—Expandable microspheres, e.g. Expancel®
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J2303/04—Starch derivatives
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Abstract
本發明提供一種熱膨脹性微膠囊及使用該熱膨脹性微膠囊之發泡成形用組成物,該熱膨脹性微膠囊具有優異之耐熱性,並且發泡倍率高,可製造輕量且硬度高、物性(耐磨耗性)優異之成形體。
本發明係一種熱膨脹性微膠囊,其係在由聚合物構成之殼中內包有作為核劑之揮發性膨脹劑者,上述殼含有使含有含羰基單體之單體組成物聚合而成之聚合物及二氧化矽,於經進行IR光譜分析之情形時,殼中基於C=O鍵之峰強度與基於二氧化矽之峰強度的比(基於C=O鍵之峰強度/基於二氧化矽之峰強度)為0.25~1.0,最大發泡溫度(Tmax)為180~225℃。
Description
本發明係關於一種熱膨脹性微膠囊及使用該熱膨脹性微膠囊之發泡成形用組成物。
此前,為了樹脂材料之輕量化或高功能化而使用發泡劑使材料發泡,作為此種發泡劑,一般使用熱膨脹性微膠囊或化學發泡劑。
作為熱膨脹性微膠囊,熱塑性殼聚合物之中內包有液狀揮發性膨脹劑者廣為人知,該液狀揮發性膨脹劑於殼聚合物之軟化點以下之溫度下成為氣體狀。例如專利文獻1中揭示有如下方法:藉由將低沸點之脂肪族烴等揮發性膨脹劑與單體混合而形成油性混合液,於含有分散劑之水系分散介質中一面攪拌一面一同添加該油性混合液與油溶性聚合觸媒,進行懸浮聚合,而製造內包有揮發性膨脹劑之熱膨脹性微膠囊。
[先前技術文獻]
[專利文獻]
專利文獻1:日本特公昭42-26524號公報
[發明所欲解決之課題]
然而,藉由該方法獲得之熱膨脹性微膠囊由於內包有為液體成分之揮發性膨脹劑,故而根據貯存方法不同,而存在揮發性膨脹劑漏出而招致貯存穩定性變差之情況,其結果為,存在招致發泡倍率降低之情況。
又,化學發泡劑若達到分解溫度時,則會產生大量氣體,因此可提高成形品之發泡倍率,但會因氣體而導致外觀變差,或氣泡成為連續氣泡而導致成形品之硬度不必要地降低。另一方面,熱膨脹性微膠囊雖然不會使成形品之外觀受損,但發泡倍率有限。
對此,進行了如下操作:藉由併用熱膨脹性微膠囊與化學發泡劑,而製成兼具兩者優點之發泡劑。然而,於併用化學發泡劑之情形時,無法使如上所述產生之氣體留在系統內,存在氣泡成為連續氣泡,或產生空隙或漏氣之情況。其結果為,存在所獲得之發泡成形體強度降低之問題。
本發明之目的在於提供一種熱膨脹性微膠囊及使用該熱膨脹性微膠囊之發泡成形用組成物,該熱膨脹性微膠囊具有優異之耐熱性,並且發泡倍率高,可製造輕量且硬度高、耐磨耗性等物性優異之成形體。
[解決課題之技術手段]
本發明係一種熱膨脹性微膠囊,其係在由聚合物構成之殼中內包有作為核劑之揮發性膨脹劑者,上述殼含有使含有含羰基單體之單體組成物聚合而成之聚合物及二氧化矽,於經進行IR光譜分析之情形時,殼中基於C=O鍵之峰強度與基於二氧化矽之峰強度的比(基於C=O鍵之峰強度/基於二氧化矽之峰強度)為0.25~1.0,最大發泡溫度(Tmax)為180~225℃。
以下詳細敍述本發明。
本發明人等進行了努力研究,結果發現,熱膨脹性微膠囊中含有之二氧化矽與所獲得之成形體之性能有重大關聯。又,發現藉由將殼中之C=O鍵與二氧化矽設為規定之關係,可獲得具有優異之耐熱性並且發泡倍率高、可製造輕量且硬度高、物性(耐磨耗性)優異之成形體的熱膨脹性微膠囊,從而完成了本發明。
進而,本發明之熱膨脹性微膠囊於製成多粒子之集合體時流動性亦優異,故而可於例如成形時自加料斗等穩定地投入。
本發明之熱膨脹性微膠囊於經進行IR光譜分析之情形時,殼中基於C=O鍵之峰強度與基於二氧化矽之峰強度的比(基於C=O鍵之峰強度/基於二氧化矽之峰強度)為0.25~1.0。藉此,可製造輕量且硬度高、物性(耐磨耗性)優異之成形體。
又,於將本發明之熱膨脹性微膠囊與化學發泡劑併用之情形時,亦可發揮作為成核劑之作用,可使其成為化學發泡劑分解並變成氣泡之起點。上述峰比之較佳之下限為0.4,更佳之下限為0.5,進而較佳之下限為0.6,進而更佳之下限為0.7,較佳之上限為0.95,更佳之上限為0.9,進而較佳之上限為0.85,進而更佳之上限為0.8。
再者,上述IR光譜分析係指利用紅外吸收分光法所進行之吸收光譜之測定,例如可藉由IR測定器而測定。
又,上述基於C=O鍵之峰係於1700~1730 cm-1
附近出現者,上述基於二氧化矽之峰係於1100~1120 cm-1
附近出現者。
本發明之熱膨脹性微膠囊之最大發泡溫度(Tmax)的下限為180℃,上限為225℃。藉由設為上述範圍內,耐熱性變高,於在高溫區域成形含有熱膨脹性微膠囊之組成物時,可防止熱膨脹性微膠囊破裂、收縮。又,可抑制成形時之熱膨脹性微膠囊彼此之凝聚,使外觀良好。更佳之下限為185℃,進而較佳之下限為190℃,更佳之上限為222℃,進而較佳之上限為220℃。
再者,於本說明書中,最大發泡溫度意指一面將熱膨脹性微膠囊自常溫起加熱一面測定其直徑時熱膨脹性微膠囊之直徑成為最大時(最大位移量)之溫度。
又,發泡起始溫度(Ts)之較佳之上限為170℃。藉由設為170℃以下,發泡變得容易,可實現期望之發泡倍率。較佳之下限為145℃,更佳之上限為165℃。
進而,本發明之熱膨脹性微膠囊利用熱機械分析而測得之最大位移量(Dmax)之較佳之下限為350 μm,較佳之上限為1000 μm。藉由設為上述範圍內,發泡倍率提昇,可獲得期望之發泡性能。再者,上述最大位移量係指一面將規定量之熱膨脹性微膠囊自常溫起加熱一面測定其直徑時規定量整體之熱膨脹性微膠囊之直徑成為最大時之值。
本發明之熱膨脹性微膠囊之平均粒徑(體積平均粒徑)的較佳之下限為10 μm,較佳之上限為35 μm。藉由設為上述範圍內,所獲得之成形體之氣泡變得適度,可獲得充分的發泡倍率,可製成外觀方面亦優異者。更佳之下限為15 μm,進而較佳之下限為20 μm,更佳之上限為30 μm,進而較佳之上限為25 μm。
又,本發明之熱膨脹性微膠囊之體積平均粒徑的CV值較佳為35%以下,通常為10%以上,較佳為15%以上。
構成本發明之熱膨脹性微膠囊之殼含有聚合物及二氧化矽,該聚合物係使含有自由基聚合性不飽和羧酸單體之單體組成物聚合而成。
上述殼含有二氧化矽。
上述二氧化矽可附著於上述殼之表面,亦可混合存在於殼內。再者,上述二氧化矽亦包含二氧化矽之水合物。
作為上述二氧化矽,可列舉含有於矽石微粒子中者或含有於矽酸膠中者等。
上述矽酸膠為二氧化矽或二氧化矽之水合物之膠體。
作為含有上述二氧化矽之矽酸膠,較佳為平均粒徑為10~300 nm。
上述殼含有使含有含羰基單體之單體組成物聚合而成之聚合物及二氧化矽。
作為上述含羰基單體,可列舉:上述碳數為3~8之自由基聚合性不飽和羧酸單體、碳數為3~8之自由基聚合性不飽和羧酸酯單體、多官能性羧酸酯單體等。
作為上述碳數為3~8之自由基聚合性不飽和羧酸單體,例如可使用每個分子中具有1個用以使其進行離子交聯之游離羧基者。
具體而言,例如可列舉不飽和羧酸或其無水物,其等可單獨使用,亦可併用2種以上。
作為上述不飽和羧酸,可列舉:丙烯酸、甲基丙烯酸、乙基丙烯酸、丁烯酸、桂皮酸等不飽和單羧酸,順丁烯二酸、伊康酸、反丁烯二酸、檸康酸、氯代順丁烯二酸等不飽和二羧酸。
此等之中,尤佳為丙烯酸、甲基丙烯酸、順丁烯二酸、順丁烯二酸酐、伊康酸。
上述單體組成物中之上述碳數3~8之自由基聚合性不飽和羧酸單體的含量較佳下限為5重量%,較佳上限為50重量%。藉由設為5重量%以上,可提高最大發泡溫度,藉由設為50重量%以下,可提昇發泡倍率。較佳之下限為10重量%,較佳之上限為30重量%。
作為上述碳數為3~8之自由基聚合性不飽和羧酸酯單體,例如較佳為(甲基)丙烯酸酯,尤佳為甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸正丁酯等甲基丙烯酸烷基酯類。又,較佳為甲基丙烯酸環己酯、甲基丙烯酸苄酯、甲基丙烯酸異莰酯等含脂環-芳香環-雜環之甲基丙烯酸酯類。
上述單體組成物中之上述碳數為3~8之自由基聚合性不飽和羧酸酯單體的含量較佳下限為10重量%,較佳上限為35重量%。藉由將上述碳數為3~8之自由基聚合性不飽和羧酸酯單體之含量設為10重量%以上,可提昇使用熱膨脹性微膠囊之組成物之分散性,藉由設為35重量%以下,可提昇微胞壁之阻氣性,改善熱膨脹性。上述碳數為3~8之自由基聚合性不飽和羧酸酯單體的含量更佳下限為15重量%,更佳上限為30重量%。
上述多官能性羧酸酯單體係指具有2個以上自由基聚合性雙鍵之羧酸酯單體,係與上述碳數為3~8之自由基聚合性不飽和羧酸酯單體不同者。上述多官能性羧酸酯單體具有作為交聯劑之作用。藉由含有上述多官能性羧酸酯單體,可強化殼之強度,熱膨脹時微胞壁不易破泡。
作為上述多官能性羧酸酯單體,具體而言,例如可列舉:二(甲基)丙烯酸酯、3官能以上之(甲基)丙烯酸酯等。
作為上述二(甲基)丙烯酸酯,例如可列舉:乙二醇二(甲基)丙烯酸酯、二乙二醇二(甲基)丙烯酸酯、三乙二醇二(甲基)丙烯酸酯、丙二醇二(甲基)丙烯酸酯、1,4-丁二醇二(甲基)丙烯酸酯等。又,可列舉:1,6-己二醇二(甲基)丙烯酸酯、1,9-壬二醇二(甲基)丙烯酸酯、甘油二(甲基)丙烯酸酯、三羥甲基丙烷二(甲基)丙烯酸酯、二羥甲基三環癸烷二(甲基)丙烯酸酯等。進而,亦可使用重量平均分子量為200~600之聚乙二醇之二(甲基)丙烯酸酯。
作為上述3官能之(甲基)丙烯酸酯,可列舉:三羥甲基丙烷三(甲基)丙烯酸酯、環氧乙烷改質三羥甲基丙烷三(甲基)丙烯酸酯、新戊四醇三(甲基)丙烯酸酯、三烯丙基縮甲醛三(甲基)丙烯酸酯等。又,作為上述4官能以上之(甲基)丙烯酸酯,可列舉:新戊四醇四(甲基)丙烯酸酯、二新戊四醇六(甲基)丙烯酸酯等。
此等之中,三羥甲基丙烷三(甲基)丙烯酸酯等3官能性者或聚乙二醇等2官能性之(甲基)丙烯酸酯可於以丙烯腈為主體之殼被相對均勻地實施交聯。
上述單體組成物中之上述多官能性羧酸酯單體的含量較佳下限為0.1重量%,較佳上限為1.0重量%。藉由將上述多官能性羧酸酯單體之含量設為0.1重量%以上,可充分地發揮作為交聯劑之效果,藉由將上述多官能性羧酸酯單體之含量設為1.0重量%以下,可提昇熱膨脹性微膠囊之發泡倍率。上述多官能性羧酸酯單體的含量更佳下限為0.15重量%,更佳上限為0.9重量%。
上述單體組成物較佳為除上述含羰基單體以外亦含有丙烯腈、甲基丙烯腈等腈系單體。
藉由添加上述腈系單體,可提昇殼之阻氣性。
又,除上述含羰基單體、腈系單體以外,亦可含有偏二氯乙烯、二乙烯苯、乙酸乙烯酯、苯乙烯系單體等。
上述單體組成物中之腈系單體的含量較佳下限為40重量%,較佳上限為90重量%。藉由設為40重量%以上,可提高殼之阻氣性,提昇發泡倍率。藉由設為90重量%以下,可提昇耐熱性或防止黃變。更佳之下限為50重量%,更佳之上限為80重量%。
尤其就耐熱性、發泡倍率、輕量性、硬度、耐磨耗性之觀點而言,上述單體組成物較佳含有40~90重量%之腈系單體及10~60重量%之含羰基單體。
為了使上述單體聚合,使上述單體組成物中含有聚合起始劑。
作為上述聚合起始劑,例如可適用二烷基過氧化物、二醯基過氧化物、過氧酯、過氧化二碳酸酯、偶氮化合物等。
具體而言,例如可列舉:甲基乙基過氧化物、二第三丁基過氧化物、雙異苯丙基過氧化物等二烷基過氧化物;異丁基過氧化物、苯甲醯基過氧化物、2,4-二氯苯甲醯基過氧化物、3,5,5-三甲基己醯基過氧化物等二醯基過氧化物等。
又,可列舉:過氧化異丁酸第三丁酯、過氧化異丁酸第三己酯、過氧化新癸酸第三丁酯、過氧化新癸酸第三己酯、1-環己基-1-過氧化新癸酸甲基乙基酯、1,1,3,3-過氧化新癸酸四甲基丁基酯等。
又,可列舉:過氧化新癸酸異苯丙酯、(α,α-雙-新癸醯過氧化)二異丙基苯等過氧酯;雙(4-第三丁基環己基)過氧化二碳酸酯、過氧化二碳酸二正丙酯、過氧化二碳酸二異丙酯等。
進而可列舉:二(2-乙基乙基過氧化)二碳酸酯、過氧化二碳酸二甲氧基丁基酯、二(3-甲基-3-甲氧基丁基過氧化)二碳酸酯等過氧化二碳酸酯等。
此外,可列舉:2,2'-偶氮雙異丁腈、2,2'-偶氮雙(4-甲氧基-2,4-二甲基戊腈)、2,2'-偶氮雙(2,4-二甲基戊腈)、1,1'-偶氮雙(1-環己甲腈(cyclohexanecarbonitrile))等偶氮化合物等。
構成上述殼之聚合物之重量平均分子量的較佳下限為10萬,較佳上限為200萬。若未達10萬,則存在殼之強度降低之情況,若超過200萬,則殼之強度過高,存在發泡倍率降低之情況。
上述殼可進而視需要含有穩定劑、紫外線吸收劑、抗氧化劑、抗靜電劑、難燃劑、矽烷偶合劑、著色劑等。
本發明之熱膨脹性微膠囊於上述殼中內包有作為核劑之揮發性膨脹劑。
上述揮發性膨脹劑係於構成殼之聚合物之軟化點以下的溫度成為氣體狀之物質,低沸點有機溶劑較為合適。
作為上述揮發性膨脹劑,例如可列舉:乙烷、乙烯、丙烷、丙烯、正丁烷、異丁烷、丁烯、異丁烯、正戊烷、異戊烷、新戊烷、正己烷、庚烷、石油醚、異辛烷、辛烷、癸烷、異十二烷、十二烷、十六烷等低分子量烴等。
又,可列舉:CCl3
F、CCl2
F2
、CClF3
、CClF2
-CClF2
等氟氯碳化物;四甲基矽烷、三甲基乙基矽烷、三甲基異丙基矽烷、三甲基正丙基矽烷等四烷基矽烷等。其中較佳為異丁烷、正丁烷、正戊烷、異戊烷、正己烷、異辛烷、異十二烷及其等之混合物。該等揮發性膨脹劑可單獨使用,亦可併用2種以上。
又,作為揮發性膨脹劑,亦可使用會因加熱而熱分解成為氣體狀之熱分解型化合物。
本發明之熱膨脹性微膠囊中,上述揮發性膨脹劑之中,較佳使用碳數為5以下之低沸點烴。藉由使用此種烴,可製成發泡倍率高、快速開始發泡之熱膨脹性微膠囊。
作為製造本發明之熱膨脹性微膠囊之方法,並無特別限定,例如可藉由進行如下步驟而製造:製備水性介質之步驟、使含有單體組成物及揮發性膨脹劑之油性混合液分散於水性介質中之步驟及使上述單體聚合之步驟。
作為上述單體組成物,例如可使用上述含有40~90重量%之腈系單體及10~60重量%之含羰基單體者。
於製造本發明之熱膨脹性微膠囊之情形時,首先進行製備水性介質之步驟。具體而言,例如,藉由向聚合反應容器添加水及含有二氧化矽之分散穩定劑,並視需要添加輔助穩定劑,而製備含有二氧化矽之水性分散介質。又,亦可視需要添加亞硝酸鹼金屬鹽、氯化亞錫、氯化錫、重鉻酸鉀等。
作為上述含有二氧化矽之分散穩定劑,可列舉矽酸膠。
作為上述矽酸膠,可使用膠體溶液(水分散液)之pH超過7之鹼性矽酸膠,亦可使用pH未達7之酸性矽酸膠。其中,更佳為鹼性矽酸膠。
又,作為上述矽酸膠,較佳含有10~50重量%之作為固形物成分之二氧化矽,且為單分散。
作為除上述二氧化矽以外之分散穩定劑,例如可列舉:磷酸鈣、氫氧化鎂、氫氧化鋁、氫氧化鐵、硫酸鋇、硫酸鈣、硫酸鈉、草酸鈣、碳酸鈣、碳酸鋇、碳酸鎂等。
上述含有二氧化矽之分散穩定劑之添加量根據熱膨脹性微膠囊之粒徑而適當決定,但相對於油性混合液(油相)100重量份,較佳之下限為2.5重量份,較佳之上限為7重量份。進而較佳之下限為3重量份,進而較佳之上限為5重量份。再者,上述油相之量意指單體與揮發性膨脹劑之合計量。
作為上述輔助穩定劑,例如可列舉二乙醇胺與脂肪族二羧酸之縮合產物、脲與甲醛之縮合產物等。又,可列舉:聚乙烯吡咯啶酮、聚環氧乙烷、聚伸乙基亞胺、氫氧化四甲基銨、明膠、甲基纖維素、聚乙烯醇、磺琥珀酸二辛酯(dioctyl sulfosuccinate)、山梨醇酯、各種乳化劑等。
又,作為上述分散穩定劑與輔助穩定劑之組合,並無特別限定,例如可列舉:矽酸膠與縮合產物之組合、矽酸膠與水溶性含氮化合物之組合等。此等之中,較佳為矽酸膠與縮合產物之組合。
進而,作為上述縮合產物,較佳為二乙醇胺與脂肪族二羧酸之縮合產物,尤佳為二乙醇胺與己二酸之縮合物或二乙醇胺與伊康酸之縮合產物。
作為上述水溶性含氮化合物,例如可列舉:聚乙烯吡咯啶酮、聚伸乙基亞胺、聚氧乙烯烷基胺、以聚甲基丙烯酸二甲胺基乙酯或聚丙烯酸二甲胺基乙酯為代表之聚(甲基)丙烯酸二烷基胺基烷基酯。又,可列舉:以聚二甲胺基丙基丙烯醯胺或聚二甲胺基丙基甲基丙烯醯胺為代表之聚二烷基胺基烷基(甲基)丙烯醯胺、聚丙烯醯胺、聚陽離子性丙烯醯胺、聚胺碸、聚烯丙胺等。此等之中,較適用聚乙烯吡咯啶酮。
關於上述縮合產物或水溶性含氮化合物之量,根據熱膨脹性微膠囊之粒徑而適當決定,但相對於油性混合液100重量份,較佳之下限為0.05重量份,較佳之上限為0.2重量份。
除上述分散穩定劑及輔助穩定劑以外,亦可進而添加氯化鈉、硫酸鈉等無機鹽。藉由添加無機鹽,可獲得具有更均勻粒子形狀之熱膨脹性微膠囊。上述無機鹽之添加量通常相對於單體100重量份,較佳為0~100重量份。
含有上述分散穩定劑之水性分散介質,係將分散穩定劑或輔助穩定劑摻合於去離子水中而製備,此時之水相之pH根據所使用之分散穩定劑或輔助穩定劑之種類而適當決定。例如於使用二氧化矽作為分散穩定劑之情形時,於酸性介質中進行聚合,要使水性介質為酸性,可視需要添加鹽酸等酸使系統之pH調整為3~4。另一方面,於使用氫氧化鎂或磷酸鈣之情形時,於鹼性介質之中使其聚合。
其次,於製造熱膨脹性微膠囊之方法中,進行使含有單體組成物及揮發性膨脹劑之油性混合液分散於水性介質中之步驟。
具體而言,例如進行如下步驟:使油性混合液分散於水性介質中,該油性混合液含有上述含有40~90重量%之腈系單體及10~60重量%之含羰基單體的單體組成物、以及揮發性膨脹劑。於該步驟中,可將單體組成物及揮發性膨脹劑分開添加至水性分散介質中,並於水性分散介質中製備油性混合液,但通常預先將兩者混合而製成油性混合液之後再添加至水性分散介質。此時,可藉由預先於分開之容器製備油性混合液與水性分散介質,並於另一容器中一面攪拌一面混合,而使油性混合液分散於水性分散介質之後(一次分散液)添加至聚合反應容器中。
再者,為了使上述單體聚合而使用聚合起始劑,上述聚合起始劑可預先添加至上述油性混合液中,亦可於聚合反應容器內將水性分散介質與油性混合液加以攪拌混合之後添加。
作為使含有上述單體組成物及揮發性膨脹劑之油性混合液分散於水性介質中之步驟,可舉藉由後掠葉等攪拌葉或批次式高速旋轉高剪切型分散器(例如日本特開平7-96167號)及連續式高速旋轉高剪切型分散器(例如日本特開2000-191817號)等進行攪拌之方法。又,可舉使其通過管路型混合器或靜態管內混合器(靜態混合器)等管內型分散裝置之方法等。
尤其於本發明中,於使含有上述單體組成物及揮發性膨脹劑之油性混合液分散於水性介質中之步驟中,較佳使用靜態管內混合器使其分散。藉由使用上述靜態管內混合器,可實現管內而非槽內之混合及不使用攪拌葉之靜態混合,故可較適合地製作峰強度比(基於C=O鍵之峰強度/基於二氧化矽之峰強度)為規定範圍內之熱膨脹性微膠囊。又,此時,預先於分開之容器內製備油性混合液與水性分散介質之一次分散液,於加壓之狀態下投入至靜態管內混合器。
再者,上述靜態管內混合器(靜態混合器)於兩端開口之筒狀體內安裝有形成有多個孔之多個板狀元件。又,其為如下構造:於至少一部分相鄰之多個板狀元件之間,相鄰之板狀元件之孔之中心不相互對準,但以至少彼此之開口之一部分對向之方式重疊多片。
藉由進行此種步驟,可較適合地製造本發明之熱膨脹性微膠囊。又,上述加壓較佳為於1~6 MPa進行。
又,較佳為根據流量而設定存在於元件之孔之個數。
進而,上述加壓可根據孔徑與流速而設定。上述孔徑較佳為1~3 mm。關於流速,較佳為100~500 L/min。具體而言,較佳為孔徑2 mm、流速200 L/min等之組合。
本發明之熱膨脹性微膠囊可藉由進行如下步驟而製造:藉由對經上述步驟獲得之分散液進行加熱而使單體聚合之步驟及洗淨之步驟。藉由此種方法而製造之熱膨脹性微膠囊之最大發泡溫度高,耐熱性優異,在高溫區域下成形時亦不會破裂、收縮。
於本發明之熱膨脹性微膠囊之製造方法中,進行洗淨步驟。
作為上述洗淨步驟,例如可列舉:浸漬洗淨、流水洗淨、噴淋洗淨方法等,進而可應用將該等方法與超音波或擺動加以組合之洗淨方法等。
又,上述洗淨步驟藉由與脫水步驟併用,可提昇生產效率。具體而言,可列舉以下方法。
將由壓榨脫水機供給之漿料製成濕濾餅之後,將規定量之洗淨水(較理想為離子交換水)供給至脫水機內,再次進行壓榨。再次供給洗淨水進行壓榨。將該步驟反覆進行數次。此處,供給至脫水機之漿料量與洗淨水之量或比率及洗淨次數於去除氯化鈉、硫酸鈉等無機鹽之方面至關重要。
藉由經過該步驟,可去除無機鹽,可防止半導體用途或汽車構件用途(成形用途)中之設備之腐蝕。
於本發明之熱膨脹性微膠囊添加化學發泡劑及熱塑性樹脂等基質樹脂而形成發泡成形用組成物,或藉由將熱膨脹性微膠囊及化學發泡劑與熱塑性樹脂等基礎樹脂加以混合而獲得母料顆粒。
又,將添加有熱塑性樹脂等基質樹脂之發泡成形用組成物添加至上述母料顆粒,使用射出成形等成形方法成形之後,藉由成形時之加熱使上述熱膨脹性微膠囊發泡,藉此,可製造發泡成形體。
本發明之發泡成形用組成物較佳為相對於基質樹脂100重量份,含有0.1~3.0重量份之熱膨脹性微膠囊、0.5~4.0重量份之化學發泡劑。
作為上述化學發泡劑,只要為常溫下為粉末狀者,則並無特別限定,可使用自以往就被通用作為化學發泡劑者。
上述化學發泡劑分類為有機系發泡劑與無機系發泡劑,各者進一步分類為熱分解型與反應型。
作為有機系之熱分解型發泡劑,經常使用ADCA(偶氮二甲醯胺)、DPT(N,N'-二硝基五亞甲基四胺)、OBSH(4,4'-氧代雙苯碸醯肼)等。
作為無機系之熱分解型發泡劑,有碳酸氫鹽、碳酸鹽、碳酸氫鹽與有機酸鹽之組合等。作為上述化學發泡劑,較佳使用熱分解型化學發泡劑。又,決定熱分解型化學發泡劑之性能的是分解溫度、氣體產生量、粒徑。
上述化學發泡劑之分解溫度較佳為180~200℃。
上述分解溫度可視需要將脲系或鋅系之發泡助劑等加以組合使用,藉此加以調整。
上述化學發泡劑之氣體產生量較佳為220~240 ml/g。再者,上述氣體產生量係化學發泡劑分解時產生之氣體之體積。該氣體會成為氣泡內之氣體,因此影響發泡倍率。進而,可藉由將上述化學發泡劑與檸檬酸鹽或氧化鋅併用而使氣泡徑變小。
上述化學發泡劑通常為粉末,粒徑越小,每單位重量之粒子數越多。往往粒子數越多,產生氣泡數越多。
上述化學發泡劑之平均粒徑(中值粒徑)之較佳下限為4 μm,較佳上限為20 μm。藉由設為上述範圍內,所獲得之成形體之氣泡變得適度,可獲得充分的發泡倍率,可製成外觀方面亦優異者。更佳之下限為5 μm,更佳之上限為10 μm。
於本發明之發泡成形用組成物中,熱膨脹性微膠囊之平均粒徑與化學發泡劑之平均粒徑的比(熱膨脹性微膠囊之平均粒徑/化學發泡劑之平均粒徑)較佳為1.0~7.5。化學發泡劑之粒徑小於熱膨脹性微膠囊之粒徑者之熱膨脹性微膠囊更容易成為源自化學發泡劑之氣泡生長之成核劑。
作為上述發泡成形體之成形方法,並無特別限定,例如可列舉:混練成形、壓延成形、擠出成形、射出成形等。於射出成形之情形時,方法並無特別限定,可列舉將一部分樹脂材料放入模具使其發泡之短射法,或將樹脂材料填滿模具之後打開模具直至欲使其發泡之程度為止之抽芯法等。
[發明之效果]
若根據本發明,可製成具有優異之耐熱性並且發泡倍率高、可製造輕量且硬度高、物性(耐摩耗性)優異之成形體的熱膨脹性微膠囊及使用該熱膨脹性微膠囊之發泡成形用組成物。又,本發明之熱膨脹性微膠囊可適用於汽車構件、塗料、黏著劑及油墨。
以下揭示實施例進一步詳細地對本發明之態樣進行說明,但本發明並不僅限定於該等實施例。
(實施例1)
(熱膨脹性微膠囊之製作)
將333.7重量份之固形物成分20重量%之矽酸膠(平均粒徑20 nm)、6重量份之聚乙烯吡咯啶酮、1094重量份之氯化鈉、1.0重量份之亞硝酸鈉添加至3100重量份之離子交換水並加以混合之後,製備水系分散介質。再者,作為矽酸膠(水分散液),使用鹼性矽酸膠。
將722.2重量份(43.33重量%)之丙烯腈、157.6重量份(9.46重量%)之甲基丙烯腈、415重量份(24.90重量%)之甲基丙烯酸、365.2重量份(21.912重量%)之甲基丙烯酸甲酯、6.64重量份(0.398重量%)之三羥甲基丙烷三甲基丙烯酸酯加以混合而製成均勻溶液之單體組成物(括弧內為相對於單體組成物整體之重量%)。於其中添加10重量份之2,2'-偶氮雙異丁腈、2.5重量份之2,2'-偶氮雙(2,4-二甲基戊腈)、400重量份之正戊烷,並於罐1之中添加混合。
其次,將水系分散介質添加至罐2之中,將罐1之油性混合物投入至罐2,進行混合而獲得一次分散液。此時,一次分散液之pH為3.5~4.0。使用靜態管內混合器(靜態混合器,富士金股份有限公司製造,分散君)使所獲得之一次分散液以流速200 L/min、壓力1.5 MPa通過。通過之液體添加至高壓釜中。
再者,關於所使用之元件式靜止型分散器,使用如下者:板狀元件以厚度5 mm、有效直徑15 mm、板狀元件之孔徑2 mm形成杵狀之形狀,於相鄰之不同種類之板狀元件之間至少一部分可對向之孔數為78個。並且,由第1元件與第2元件之組合構成之單元的數量為10組,以成為通過各板狀元件之孔之流體的方式設置。
其後,進行氮氣置換,於反應溫度60℃使其反應15小時。反應壓力為0.5 MPa,攪拌以200 rpm進行。
其後,將所獲得之聚合漿料8000 L分次供給至壓榨脫水裝置(石垣公司製造,壓濾機)中,脫水後將洗淨水之規定量供給至脫水機,進行洗淨步驟之後,使其乾燥,獲得熱膨脹性微膠囊。
(實施例2~6、比較例1~7)
以表1所示之組成將丙烯腈、甲基丙烯腈、甲基丙烯酸、甲基丙烯酸甲酯、三羥甲基丙烷三甲基丙烯酸酯、異戊烷、正戊烷、異辛烷、矽酸膠加以混合,製成單體組成物之後,於表1所示之乳化條件下進行乳化,除此以外,以與實施例1相同之方式獲得熱膨脹性微膠囊。其中,於甲基丙烯酸之添加量為0.1重量%之比較例1及甲基丙烯酸之添加量較少之實施例4、6及比較例2之情形時,於水系分散介質添加鹽酸以調整為pH3.5~4.0。
再者,作為普通攪拌機,使用批次式高速旋轉高剪切型分散器(M 技術股份有限公司製造,Clear mix CLM-150S,轉子R2)。
(實施例7~12、比較例8~16)
(發泡成形體之製造)
使用亨舍爾混合機(於120℃使其乾透)以表2所示之摻合進行混合,利用射出成形機(JSW公司製造,350t)使所獲得之複合物抽芯成形(樹脂溫度200℃,模具溫度40℃,抽芯量3.0 mm),藉此,獲得發泡成形體。
再者,使用鄰苯二甲酸二(2-乙基己基)酯(DOP,三菱化學公司製造)作為塑化劑,使用重質碳酸鈣(Whiton 305,白石工業公司製造)作為填充劑,使用錫系穩定劑(ONZ142AF,三共有機合成公司製造)作為熱穩定劑,使用聚乙烯蠟(AC316A,Honeywell公司製造)作為加工助劑。
(1)熱膨脹性微膠囊之評價
(1-1)體積平均粒徑、CV值
使用粒度分佈徑測定器(LΑ-950,HORIBA公司製造),測定體積平均粒徑、CV值。
(1-2)發泡起始溫度、最大發泡溫度、最大位移量
使用熱機械分析裝置(TMA)(TMA2940,TA instruments公司製造)測定發泡起始溫度(Ts)、最大位移量(Dmax)及最大發泡溫度(Tmax)。具體而言,將25 μg之試樣放入直徑7 mm、深1 mm之鋁製容器,於自上面施加0.1 N之力之狀態下,以5℃/min之升溫速度自80℃加熱至220℃,對測定端子之垂直方向上之位移進行測定,將位移開始上升之溫度設為發泡起始溫度,將該位移之最大值設為最大位移量,將最大位移量時之溫度設為最大發泡溫度。
(1-3)IR光譜分析
針對實施例及比較例中獲得之熱膨脹性微膠囊,保持封入有核劑之狀態取多個(2個以上),使用FTIR分光光度計(Thermo Scientific公司製造,Nicolet iS50)進行IR光譜分析。由(透射)IR光譜分析之結果求出殼中基於C=O鍵之峰強度(1700~1730 cm-1
附近)、基於二氧化矽之峰強度(1100~1120 cm-1
附近),算出(基於C=O鍵之峰強度/基於二氧化矽之峰強度)。再者,測定值為平均值。
(1-4)加料斗流動性
使用JIS K7370所記載之體積比重測定用容器,將所獲得之熱膨脹性微膠囊投入至加料斗之上部,其後,使其以自身重量掉落,測定加料斗變空時(熱膨脹性微膠囊全部落下時)之秒數。
(2)發泡成形體之評價
(2-1)密度
藉由依據JIS K 7112 A法(水中置換法)之方法測定所獲得之發泡成形體之密度。
(2-2)A型硬度
利用依據JIS K 6253之方法測定所獲得之發泡成形體之A型硬度。
(2-3)磨耗量
利用依據阿克隆磨耗試驗法(JIS K 6264)之方法,以負載26.5 N測定每1000轉之磨耗體積。
[表1]
實施例1 | 實施例2 | 實施例3 | 實施例4 | 實施例5 | 實施例6 | 比較例1 | 比較例2 | 比較例3 | 比較例4 | 比較例5 | 比較例6 | 比較例7 | ||
組成 (重量份) | 丙烯腈 | 43.33 | 43.33 | 43.33 | 19.93 | 43.33 | 19.93 | 69.722 | 59.762 | 43.33 | 43.33 | 43.33 | 33.33 | 43.33 |
甲基丙烯腈 | 9.46 | 9.46 | 9.46 | 29.871 | 9.46 | 29.871 | 29.78 | 9.96 | 9.46 | 9.46 | 9.46 | 9.46 | 9.46 | |
甲基丙烯酸 | 24.90 | 24.90 | 24.90 | 19.93 | 24.90 | 19.93 | 0.1 | 19.92 | 24.90 | 27.90 | 24.90 | 29.90 | 24.90 | |
甲基丙烯酸甲酯 | 21.912 | 21.912 | 21.912 | 29.871 | 21.912 | 29.871 | 0 | 9.96 | 21.912 | 18.912 | 21.912 | 26.912 | 21.912 | |
三羥甲基丙烷三甲基丙烯酸酯 | 0.398 | 0.398 | 0.398 | 0.398 | 0.398 | 0.398 | 0.398 | 0.398 | 0.398 | 0.398 | 0.398 | 0.398 | 0.398 | |
異戊烷 | - | - | 24 | 19.2 | - | 19.2 | - | - | 24 | - | - | - | - | |
正戊烷 | 24 | 24 | - | - | 24 | - | 24 | 24 | - | - | 24 | 24 | 24 | |
異辛烷 | - | - | - | 4.8 | - | 4.8 | - | - | - | 24 | - | - | - | |
矽酸膠(相對於油相100重量份之量) | 3.23 | 3.23 | 4 | 3.23 | 3.23 | 3.23 | 3.23 | 2.2 | 2.4 | 3.23 | 10.5 | 3.23 | 3.23 | |
攪拌方法 | 靜態混合器 | ○ | ○ | ○ | ○ | ○ | ○ | - | - | - | ○ | ○ | ○ | - |
普通攪拌機 | - | - | - | - | - | - | ○ | ○ | ○ | - | - | - | ○ | |
乳化時壓力(MPa) | 1.5 | 3.0 | 3 | 1.5 | 1.0 | 1.0 | 0 | 0 | 0 | 1.0 | 4 | 1.5 | 0 | |
乳化時流速(L/min) | 200 | 200 | 200 | 200 | 200 | 200 | - | - | - | 200 | 400 | 200 | - | |
評價 | 體積平均粒徑(μm) | 30 | 25 | 23 | 28 | 33.3 | 25.2 | 30.1 | 41.6 | 38.6 | 30 | 8.6 | 30 | 30 |
CV值(%) | 23 | 20 | 19 | 25 | 35 | 27 | 32 | 44 | 40 | 24 | 16 | 23 | 23 | |
[A]基於C=O鍵之峰強度 | 0.188 | 0.188 | 0.196 | 0.132 | 0.187 | 0.132 | 0.025 | 0.132 | 0.188 | 0.188 | 0.188 | 0.25 | 0.176 | |
[B]基於二氧化矽之峰強度 | 0.23 | 0.21 | 0.2 | 0.22 | 0.252 | 0.38 | 0.117 | 0.11 | 0.134 | 0.23 | 0.23 | 0.23 | 0.131 | |
[A]/[B] | 0.817 | 0.895 | 0.980 | 0.600 | 0.742 | 0.347 | 0.214 | 1.200 | 1.403 | 0.817 | 0.817 | 1.087 | 1.344 | |
發泡起始溫度(Ts)(℃) | 165 | 166 | 160 | 160 | 148 | 166 | 139 | 160 | 148 | 185 | 166 | 180 | 165 | |
最大發泡溫度(Tmax)(℃) | 215 | 220 | 208 | 221 | 188 | 219 | 173 | 221 | 188 | 232 | 177 | 225 | 215 | |
最大位移量(Dmax)(μm) | 650 | 550 | 660 | 720 | 513 | 560 | 820 | 720 | 513 | 280 | 175 | 250 | 650 | |
加料斗流動性(秒) | 20 | 18 | 17.5 | 23 | 28 | 24 | 26 | 46 | 41 | 20 | 49 | 21 | 20 |
[表2]
[產業上之可利用性]
實施例7 | 實施例8 | 實施例9 | 實施例10 | 實施例11 | 實施例12 | 比較例8 | 比較例9 | 比較例10 | 比較例11 | 比較例12 | 比較例13 | 比較例14 | 比較例15 | 比較例16 | |||
摻合 | 樹脂 | 類別 | PVC | PVC | PVC | PVC | PVC | PVC | PVC | PVC | PVC | PVC | PVC | PVC | PVC | PVC | PVC |
添加量[重量%] | 49.0 | 49.0 | 49.0 | 49.0 | 49.0 | 49.0 | 49.0 | 49.0 | 49.0 | 49.0 | 49.0 | 49.0 | 49.0 | 49.0 | 49.0 | ||
熱膨脹性 微膠囊 | 類別 | 實施例1 | 實施例2 | 實施例3 | 實施例4 | 實施例5 | 實施例6 | 比較例1 | 比較例2 | 比較例3 | 比較例3 | 比較例4 | 比較例5 | 比較例6 | 比較例7 | 比較例2 | |
添加量[重量%] | 0.5 | 0.5 | 0.5 | 0.5 | 1.0 | 1.0 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | ||
化學發泡劑 | 類別 | ADCA | ADCA | ADCA | ADCA | ADCA | ADCA | ADCA | ADCA | ADCA | ADCA | ADCA | ADCA | ADCA | ADCA | ADCA | |
添加量[重量%] | 1.0 | 1.0 | 1.0 | 1.0 | 0.5 | 0.5 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | 1.0 | ||
平均粒徑(μm) | 6 | 8 | 4 | 4 | 8 | 8 | 8 | 8 | 8 | 20 | 6 | 6 | 6 | 6 | 4 | ||
粒徑比(微膠囊/化學發泡劑) | 5.00 | 3.125 | 5.75 | 7.00 | 4.16 | 4.16 | 3.76 | 5.20 | 4.83 | 1.93 | 5.00 | 5.00 | 5.00 | 5.00 | 10.40 | ||
塑化劑添加量[重量%] | 37.00 | 37.00 | 37.00 | 37.00 | 37.00 | 37.00 | 37.00 | 37.00 | 37.00 | 37.00 | 37.00 | 37.00 | 37.00 | 37.00 | 37.00 | ||
填充劑添加量[重量%] | 10.00 | 10.00 | 10.00 | 10.00 | 10.00 | 10.00 | 10.00 | 10.00 | 10.00 | 10.00 | 10.00 | 10.00 | 10.00 | 10.00 | 10.00 | ||
熱穩定劑添加量[重量%] | 2.00 | 2.00 | 2.00 | 2.00 | 2.00 | 2.00 | 2.00 | 2.00 | 2.00 | 2.00 | 2.00 | 2.00 | 2.00 | 2.00 | 2.00 | ||
加工助劑添加量[重量%] | 0.50 | 0.50 | 0.50 | 0.50 | 0.50 | 0.50 | 0.50 | 0.50 | 0.50 | 0.50 | 0.50 | 0.50 | 0.50 | 0.50 | 0.50 | ||
評價 | 成形品 | 密度(g/cm3 ) | 0.44 | 0.42 | 0.405 | 0.403 | 0.49 | 0.48 | 0.473 | 0.478 | 0.469 | 0.485 | 0.491 | 0.490 | 0.492 | 0.485 | 0.415 |
A型硬度 | 35.50 | 36.80 | 38.10 | 39.50 | 34.50 | 35.00 | 29.5 | 33.40 | 34.40 | 29.00 | 28.50 | 27.50 | 28.80 | 30.00 | 28.50 | ||
磨耗量(ml) | 120 | 115 | 80 | 80 | 120 | 118 | 230 | 200 | 190 | 250 | 260 | 280 | 280 | 245 | 255 |
若根據本發明,可提供一種具有優異之耐熱性並且發泡倍率高、可製造輕量且硬度高、物性(耐磨耗性)優異之成形體的熱膨脹性微膠囊及使用該熱膨脹性微膠囊之發泡成形用組成物。
無
無
Claims (5)
- 一種熱膨脹性微膠囊,其係在由聚合物構成之殼中內包有揮發性膨脹劑作為核劑者,該殼含有使含有含羰基單體之單體組成物聚合而成之聚合物及二氧化矽,該含羰基單體含有碳數為3~8之自由基聚合性不飽和羧酸酯單體及碳數為3~8之自由基聚合性不飽和羧酸單體,該單體組成物中之碳數為3~8之自由基聚合性不飽和羧酸酯單體之含量為10重量%以上35重量%以下,該碳數為3~8之自由基聚合性不飽和羧酸單體之含量為5重量%以上50重量%以下,於經進行IR光譜分析之情形時,殼中基於C=O鍵之峰強度與基於二氧化矽之峰強度的比(基於C=O鍵之峰強度/基於二氧化矽之峰強度)為0.25~1.0,最大發泡溫度(Tmax)為180~225℃。
- 如請求項1之熱膨脹性微膠囊,其平均粒徑為10~30μm。
- 一種發泡成形用組成物,其含有請求項1或2之熱膨脹性微膠囊、化學發泡劑及基質樹脂。
- 如請求項3之發泡成形用組成物,其相對於基質樹脂100重量份含有0.1~3.0重量份之熱膨脹性微膠囊、0.5~4.0重量份之化學發泡劑。
- 如請求項3或4之發泡成形用組成物,其中,熱膨脹性微膠囊之平均粒徑與化學發泡劑之平均粒徑的比(熱膨脹性微膠囊之平均粒徑/化學發泡劑之平均粒徑)為1.0~7.5。
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JP2023134426A (ja) | 2023-09-27 |
WO2020158613A1 (ja) | 2020-08-06 |
CN113272341A (zh) | 2021-08-17 |
EP3892654A1 (en) | 2021-10-13 |
EP3892654A4 (en) | 2022-08-17 |
JPWO2020158613A1 (ja) | 2021-12-09 |
US20220119614A1 (en) | 2022-04-21 |
JP7296946B2 (ja) | 2023-06-23 |
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