TW202313822A - 成核劑組成物、樹脂組成物、其成型品及樹脂組成物之製造方法 - Google Patents
成核劑組成物、樹脂組成物、其成型品及樹脂組成物之製造方法 Download PDFInfo
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- TW202313822A TW202313822A TW111122420A TW111122420A TW202313822A TW 202313822 A TW202313822 A TW 202313822A TW 111122420 A TW111122420 A TW 111122420A TW 111122420 A TW111122420 A TW 111122420A TW 202313822 A TW202313822 A TW 202313822A
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- 239000000203 mixture Substances 0.000 title claims abstract description 72
- 239000011342 resin composition Substances 0.000 title claims abstract description 72
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- 239000013078 crystal Substances 0.000 claims abstract description 74
- 229920005672 polyolefin resin Polymers 0.000 claims abstract description 73
- 238000001938 differential scanning calorimetry curve Methods 0.000 claims abstract description 44
- 238000000113 differential scanning calorimetry Methods 0.000 claims abstract description 30
- -1 carboxylate salts Chemical class 0.000 claims description 75
- 229910052751 metal Inorganic materials 0.000 claims description 35
- 239000002184 metal Substances 0.000 claims description 35
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- 239000003484 crystal nucleating agent Substances 0.000 claims description 29
- 238000002156 mixing Methods 0.000 claims description 21
- 238000000465 moulding Methods 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 16
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 14
- 229920005989 resin Polymers 0.000 claims description 14
- 239000011347 resin Substances 0.000 claims description 14
- 230000015572 biosynthetic process Effects 0.000 claims description 13
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- 238000004364 calculation method Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
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- 239000008116 calcium stearate Substances 0.000 claims description 9
- 235000013539 calcium stearate Nutrition 0.000 claims description 9
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 claims description 9
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- NRCMAYZCPIVABH-UHFFFAOYSA-N Quinacridone Chemical class N1C2=CC=CC=C2C(=O)C2=C1C=C1C(=O)C3=CC=CC=C3NC1=C2 NRCMAYZCPIVABH-UHFFFAOYSA-N 0.000 claims description 4
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 2
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- ZHROMWXOTYBIMF-UHFFFAOYSA-M sodium;1,3,7,9-tetratert-butyl-11-oxido-5h-benzo[d][1,3,2]benzodioxaphosphocine 11-oxide Chemical compound [Na+].C1C2=CC(C(C)(C)C)=CC(C(C)(C)C)=C2OP([O-])(=O)OC2=C1C=C(C(C)(C)C)C=C2C(C)(C)C ZHROMWXOTYBIMF-UHFFFAOYSA-M 0.000 description 1
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Abstract
本發明係提供一種可賦予包含聚烯烴系樹脂之成型品優良的力學的特性成核劑組成物、包含其之樹脂組成物、具有優良力學的特性之其成型品及樹脂組成物之製造方法。
其係一種成核劑組成物,其特徵在於,其中包含至少一種聚烯烴系樹脂用成核劑,且藉由以下之方法所算出之β晶分率為0.2~71%。使用由包含成核劑組成物之樹脂組成物之團塊所取樣之試料,並藉由特定的程序來進行示差掃描熱量測定,並將橫軸設為溫度θ(℃)、縱軸設為熱流量Q(mW)求出DSC曲線Q=f(θ)、基準線g(θ),獲得經基準線補正之DSC曲線Q’=h(θ)=f(θ)-g(θ)。然後,依據特定的步驟,求取線面積S
t與β晶之面積S
β,算出β晶分率(%)。
β晶分率=S
β/S
t×100(%)
Description
本發明係關於成核劑組成物、樹脂組成物、其成型品及樹脂組成物之製造方法,詳細而言,係關於可賦予包含聚烯烴系樹脂之成型品優良的力學的特性成核劑組成物、包含其之樹脂組成物、具有優良力學的特性之其成型品及樹脂組成物之製造方法。
聚烯烴系樹脂,在各種熱可塑性通用樹脂中,就物性、成型加工性、價格等的點而言,係作為應用領域最廣之塑膠材料之一而被使用於廣泛的用途中。
由聚烯烴系樹脂構成之成型品係常被要求具有優良的力學的特性。已知,於聚烯烴系樹脂中添加成核劑之方法,係作為對於由聚烯烴系樹脂構成之成型品賦予優良的力學的特性之方法之一。作為於聚烯烴系樹脂中添加之成核劑,例如於下述專利文獻1中,係提案出一種包含芳香族磷酸酯金屬鹽與醯胺化合物之成核劑。
[先前技術文獻]
[專利文獻]
[專利文獻1] 日本特開2008-120931號公報
[發明所欲解決之課題]
然而,上述專利文獻1中記載之成核劑,在對於成型品賦予充分的力學的特性之觀點中,仍有進一步改善的餘地。
因此,本發明之目的在於提供一種可賦予包含聚烯烴系樹脂之成型品優良的力學的特性成核劑組成物、包含其之樹脂組成物、具有優良力學的特性之其成型品及樹脂組成物之製造方法。
[用於解決課題之手段]
本發明人等,為了解決上述課題而進行積極檢討之結果,發現藉由一種成核劑組成物係可解決上述課題,而該成核劑組成物係於特定的聚烯烴系樹脂中添加特定量之該成核劑組成物時,聚烯烴系樹脂之β晶分率係介於特定之範圍,進而完成本發明。
亦即,本發明之成核劑組成物,其係特徵在於其中包含至少一種聚烯烴系樹脂用成核劑,且藉由以下之方法所算出之β晶分率為0.2~71%者。
<β晶分率之算出方法>
(1)依據JIS K 7210,摻合以溫度230℃、荷重2.16kg之條件所測定出之熔體流動速率為8g/10分之均聚聚丙烯100質量份、前述成核劑組成物0.10質量份、四[亞甲基-3-(3’,5’-tert-丁基-4’-羥基苯基)丙酸酯]甲烷0.05質量份、三(2,4-二-tert-丁基苯基)亞磷酸酯)0.1質量份及硬脂酸鈣0.05質量份,使用FM混合機混合1分鐘,獲得樹脂摻合物。
(2)使用雙軸擠壓機,將前述樹脂摻合物以熔融溫度230℃進行熔融混練,並將所獲得之熔融混練物進行造粒,獲得團塊。
(3)在使前述團塊以80℃乾燥8小時後,由乾燥後之團塊取樣出10mg之試料,導入示差掃描熱量測定裝置中。
(4)使用前述示差掃描熱量測定裝置,將前述試料以自25℃起以50℃/min之速度昇溫至230℃為止,於230℃下保持20分鐘後,以100℃/min之速度冷卻至50℃為止,並於50℃下保持20分鐘後,以30℃/min之速度昇溫至230℃為止之溫度程序來進行示差掃描熱量測定,並將橫軸設為溫度θ(℃)、縱軸設為熱流量Q(mW),獲得DSC曲線Q=f(θ)。此處,針對縱軸,係將吸熱設為正的方向。
(5)於前述DSC曲線之對應於前述溫度程序中之第2次之昇溫過程之部分中,由f(θ)將基準線g(θ)=(f(200)-f(110))/90×(θ-110)+f(110)扣除,獲得經基準線補正之DSC曲線Q’=h(θ)=f(θ)-g(θ)。
(6)將由曲線Q’=h(θ)之110≦θ≦200之部分及連結點A(110,0)及點B(200,0)之線段AB所包圍之領域之面積設為S
t。此處,S
t係以下述公式表示。
(7)將曲線Q’=h(θ)上之110≦θ≦200之範圍中之2個極大點設為R(θ
β,h(θ
β)),S(θ
α,h(θ
α))(惟θ
β<θ
α),並將曲線Q’=h(θ)上之θ
β<θ<θ
α之範圍中之極小點設為C(θ
γ,h(θ
γ)。然後,通過點C,拉出與曲線Q’=h(θ)在110<θ<θ
β之範圍內相接觸之切線,並將接點設為點D(θ
δ,h(θ
δ)。然後,係將由曲線Q’=h(θ)之θ
δ≦θ≦θ
γ之部分及連結點D及點C之線段DC所包圍之領域之面積設為S
β。
此處,S
β係以下述公式表示。
惟,j(θ)=h(θ)-i(θ),i(θ)=(h(θ
γ)-h(θ
δ))/(θ
γ-θ
δ)×(θ-θ
γ)+ h(θ
γ)。
(8)由前述S
t及前述S
β,藉由下述公式來算出β晶分率(%)。
β晶分率=S
β/S
t×100(%)
本發明之成核劑組成物中,較佳係包含促進聚烯烴系樹脂之α晶形成之α晶成核劑。
又,本發明之成核劑組成物中,較佳係包含促進聚烯烴系樹脂之β晶形成之β晶成核劑,前述β晶成核劑更佳係包含由羧酸金屬鹽及喹吖酮化合物所成之群所選出之至少一種。
又,本發明之樹脂組成物之特徵在於,其係包含聚烯烴系樹脂,及至少一種聚烯烴系樹脂用成核劑,且藉由以下之方法所算出之β晶分率為0.2~71%者。
<β晶分率之算出方法>
(1)在使前述樹脂組成物於80℃下乾燥8小時後,由乾燥後之團塊取樣出10mg之試料,導入示差掃描熱量測定裝置中。
(2)使用前述示差掃描熱量測定裝置,將前述試料以自25℃起以50℃/min之速度昇溫至230℃為止,於230℃下保持20分鐘後,以100℃/min之速度冷卻至50℃為止,並於50℃下保持20分鐘後,以30℃/min之速度昇溫至230℃為止之溫度程序來進行示差掃描熱量測定,並將橫軸設為溫度θ(℃)、縱軸設為熱流量Q(mW),獲得DSC曲線Q=f(θ)。此處,針對縱軸,係將吸熱設為正的方向。
(3)於前述DSC曲線之對應於前述溫度程序中之第2次之昇溫過程之部分中,由f(θ)將基準線g(θ)=(f(200)-f(110))/90×(θ-110)+f(110)扣除,獲得經基準線補正之DSC曲線Q’=h(θ)=f(θ)-g(θ)。
(4)將由曲線Q’=h(θ)之110≦θ≦200之部分及連結點A(110,0)及點B(200,0)之線段AB所包圍之領域之面積設為S
t。此處,S
t係以下述公式表示。
(5)將曲線Q’=h(θ)上之110≦θ≦200之範圍中之2個極大點設為R(θ
β,h(θ
β)),S(θ
α,h(θ
α))(惟θ
β<θ
α),並將曲線Q’=h(θ)上之θ
β<θ<θ
α之範圍中之極小點設為C(θ
γ,h(θ
γ)。然後,通過點C,拉出與曲線Q’=h(θ)在110<θ<θ
β之範圍內相接觸之切線,並將接點設為點D(θ
δ,h(θ
δ)。然後,係將由曲線Q’=h(θ)之θ
δ≦θ≦θ
γ之部分及連結點D及點C之線段DC所包圍之領域之面積設為S
β。
此處,S
β係以下述公式表示。
惟,j(θ)=h(θ)-i(θ),i(θ)=(h(θ
γ)-h(θ
δ))/(θ
γ-θ
δ)×(θ-θ
γ)+ h(θ
γ)。
(6)由前述S
t及前述S
β,藉由下述公式來算出β晶分率(%)。
β晶分率=S
β/S
t×100(%)
本發明之樹脂組成物中,較佳係包含促進聚烯烴系樹脂之α晶形成之α晶成核劑。
又,本發明之樹脂組成物中,較佳係包含促進聚烯烴系樹脂之β晶形成之β晶成核劑,前述β晶成核劑更佳係包含由羧酸金屬鹽及喹吖酮化合物所成之群所選出之至少一種。
此外,本發明之成型品之特徵在於,其係將上述之樹脂組成物成型而獲得者。
另外,本發明之樹脂組成物之製造方法之特徵係在於,其係包含將至少一種聚烯烴系樹脂用成核劑,以使藉由以下之方法所算出之β晶分率成為0.2~71%的方式,摻合於聚烯烴系樹脂中之摻合步驟者。
<β晶分率之算出方法>
(1)在使前述樹脂組成物於80℃下乾燥8小時後,由乾燥後之團塊取樣出10mg之試料,導入示差掃描熱量測定裝置中。
(2)使用前述示差掃描熱量測定裝置,將前述試料以自25℃起以50℃/min之速度昇溫至230℃為止,於230℃下保持20分鐘後,以100℃/min之速度冷卻至50℃為止,並於50℃下保持20分鐘後,以30℃/min之速度昇溫至230℃為止之溫度程序來進行示差掃描熱量測定,並將橫軸設為溫度θ(℃)、縱軸設為熱流量Q(mW),獲得DSC曲線Q=f(θ)。此處,針對縱軸,係將吸熱設為正的方向。
(3)於前述DSC曲線之對應於前述溫度程序中之第2次之昇溫過程之部分中,由f(θ)將基準線g(θ)=(f(200)-f(110))/90×(θ-110)+f(110)扣除,獲得經基準線補正之DSC曲線Q’=h(θ)=f(θ)-g(θ)。
(4)將由曲線Q’=h(θ)之110≦θ≦200之部分及連結點A(110,0)及點B(200,0)之線段AB所包圍之領域之面積設為S
t。此處,S
t係以下述公式表示。
(5)將曲線Q’=h(θ)上之110≦θ≦200之範圍中之2個極大點設為R(θ
β,h(θ
β)),S(θ
α,h(θ
α))(惟θ
β<θ
α),並將曲線Q’=h(θ)上之θ
β<θ<θ
α之範圍中之極小點設為C(θ
γ,h(θ
γ)。然後,通過點C,拉出與曲線Q’=h(θ)在110<θ<θ
β之範圍內相接觸之切線,並將接點設為點D(θ
δ,h(θ
δ)。然後,係將由曲線Q’=h(θ)之θ
δ≦θ≦θ
γ之部分及連結點D及點C之線段DC所包圍之領域之面積設為S
β。
此處,S
β係以下述公式表示。
惟,j(θ)=h(θ)-i(θ),i(θ)=(h(θ
γ)-h(θ
δ))/(θ
γ-θ
δ)×(θ-θ
γ)+ h(θ
γ)。
(6)由前述S
t及前述S
β,藉由下述公式來算出β晶分率(%)。
β晶分率=S
β/S
t×100(%)
[發明之效果]
依據本發明,可提供一種可賦予包含聚烯烴系樹脂之成型品優良的力學的特性成核劑組成物、包含其之樹脂組成物、具有優良力學的特性之其成型品及樹脂組成物之製造方法。
以下,係針對本發明之實施形態進行詳細的說明。首先,針對本實施形態之成核劑組成物進行說明。
<成核劑組成物>
本實施形態之成核劑組成物係包含至少一種聚烯烴系樹脂用成核劑,且藉由以下之方法所算出之β晶分率為0.2~71%。
<β晶分率之算出方法>
(1)依據JIS K 7210,摻合以溫度230℃、荷重2.16kg之條件所測定出之熔體流動速率為8g/10分之均聚聚丙烯100質量份、成核劑組成物0.10質量份、四[亞甲基-3-(3’,5’-tert-丁基-4’-羥基苯基)丙酸酯]甲烷0.05質量份、三(2,4-二-tert-丁基苯基)亞磷酸酯)0.1質量份及硬脂酸鈣0.05質量份,並使用FM混合機混合1分鐘,獲得樹脂摻合物。
(2)使用雙軸擠壓機,將樹脂摻合物於熔融溫度230℃下進行熔融混練,並將所獲得之熔融混練物進行造粒,獲得團塊。
(3)使團塊於80℃下乾燥8小時後,由乾燥後之團塊取樣出10mg之試料,導入示差掃描熱量測定裝置中。
(4)使用示差掃描熱量測定裝置,將試料以自25℃起以50℃/min之速度昇溫至230℃為止,於230℃下保持20分鐘後,以100℃/min之速度冷卻至50℃為止,於50℃下保持20分鐘後,以30℃/min之速度昇溫至230℃為止之溫度程序來進行示差掃描熱量測定,並將橫軸設為溫度θ(℃)、縱軸設為熱流量Q(mW),獲得DSC曲線Q=f(θ)。此處,針對縱軸,係將吸熱設為正的方向。
(5)於DSC曲線之對應於上述溫度程序中之第2次之昇溫過程之部分中,由f(θ)將基準線g(θ)=(f(200)-f(110))/90×(θ-110)+f(110)扣除,獲得經基準線補正之DSC曲線Q’=h(θ)=f(θ)-g(θ)。
(6)將由曲線Q’=h(θ)之110≦θ≦200之部分及連結點A(110,0)及點B(200,0)之線段AB所包圍之領域之面積設為S
t。此處,S
t係以下述公式表示。
(7)將曲線Q’=h(θ)上之110≦θ≦200之範圍中之2個極大點設為R(θ
β,h(θ
β)),S(θ
α,h(θ
α))(惟θ
β<θ
α),並將曲線Q’=h(θ)上之θ
β<θ<θ
α之範圍中之極小點設為C(θ
γ,h(θ
γ)。然後,通過點C,拉出與曲線Q’=h(θ)在110<θ<θ
β之範圍內相接觸之切線,並將接點設為點D(θ
δ,h(θ
δ)。然後,係將由曲線Q’=h(θ)之θ
δ≦θ≦θ
γ之部分及連結點D及點C之線段DC所包圍之領域之面積設為S
β。
此處,S
β係以下述公式表示。
惟,j(θ)=h(θ)-i(θ),i(θ)=(h(θ
γ)-h(θ
δ))/(θ
γ-θ
δ)×(θ-θ
γ)+ h(θ
γ)。
(8)由S
t及S
β,藉由下述公式來算出β晶分率(%)。
β晶分率=S
β/S
t×100(%)
圖1係針對後述之實施例之添加了成核劑組成物2之樹脂組成物,在示差掃描熱量測定中所獲得之DSC曲線Q=f(θ)之對應於第2次之昇溫過程之部分之曲線圖,圖2係針對實施例之添加了成核劑組成物2之樹脂組成物,將DSC曲線Q=f(θ)之對應於第2次之昇溫過程之部分進行基準線補正後之DSC曲線Q’=h(θ)=f(θ)-g(θ)之曲線圖。亦即,β晶分率(%)係意指相對於被110℃~200℃之範圍中之曲線Q’與線段AB包圍之領域面積S
t,被曲線Q’與線段CD包圍之領域面積S
β之比例。
依據本實施形態之成核劑組成物,則可賦予包含聚烯烴系樹脂之成型品優良的力學的特性。
如同上述,本實施形態之成核劑組成物中,以上述之方法所算出之β晶分率為0.2~71%。由賦予成型品更加優良的力學的特性之觀點來看,β晶分率較佳為0.3~70.0%,更佳為3.0~45.0%,再更佳為5.0~30.0%,又再進一步更佳為10.0~25.0%。
β晶分率,例如,可藉由適宜地選擇成核劑組成物中所包含之聚烯烴系樹脂用成核劑之種類及摻合比例等來控制。
作為本實施形態之成核劑組成物中所包含之聚烯烴系樹脂用成核劑,例如,可舉出促進聚烯烴系樹脂之α晶形成之α晶成核劑、促進聚烯烴系樹脂之β晶形成之β晶成核劑等。
作為α晶成核劑,例如可舉出下述一般式(1)所表示之芳香族磷酸酯金屬鹽、下述一般式(2)所表示之脂環式二羧酸金屬鹽、安息香酸鈉、4-tert-丁基安息香酸鋁等的芳香族羧酸金屬鹽、己二酸鈉等的脂肪族羧酸金屬鹽、下述一般式(3)所表示之丁二酮化合物等。
此處,一般式(1)中,R
1~R
5係各自獨立表示氫原子或碳原子數1~6之烷基,n係表示1或2,n為1之情況中,M
1係表示鹼金屬或二羥基鋁,n為2之情況中,M
1係表示鹼土類金屬、鋅或羥基鋁。
此處,一般式(2)中,R
6~R
15係各自獨立表示氫原子或碳原子數1~6之烷基,p係表示1或2,p為1之情況中,q為2,M
2係表示鹼金屬或二羥基鋁,p為2之情況中,q為1,M
2係表示鹼土類金屬、鋅或羥基鋁。R
6及R
13亦可互相連結形成環構造。
此處,一般式(3)中,R
16係表示氫原子或碳原子數1~6之烷基。R
17~R
20係各自獨立地表示氫原子、鹵素原子、氰基、碳原子數1~6之烷基或碳原子數1~6之烷氧基,或者R
17及R
18或R
19及R
20係互相連結表示碳原子數3~6之伸烷基或碳原子數1~4之伸烷基二氧基。X係表示單鍵、-CH(OH)-基或-CH(OH)CH(OH)-基。
一般式(1)中,作為R
1~R
5所表示之碳原子數1~6之烷基,例如,可舉出甲基、乙基、n-丙基、異丙基、環丙基、n-丁基、sec-丁基、tert-丁基、異丁基、環丁基、n-戊基、tert-戊基、環戊基、n-己基、環己基等。由對於成型品,賦予更優良的力學的特性之觀點來看,R
1~R
4特佳為tert-丁基。又,對於成型品,由賦予再更優良的力學的特性之觀點來看,R
5較佳為氫原子或甲基,特佳為氫原子。
M
1表示鹼金屬之情況中,作為鹼金屬,例如可舉出鋰、鈉、鉀等。此等之中,較佳為鋰、鈉,特佳為鈉。又,M
1表示鹼土類金屬之情況中,作為鹼土類金屬,例如可舉出鎂、鈣、鋇等。
對於成型品,由賦予再更優良的力學的特性之觀點來看,n較佳為1。
作為一般式(1)所表示之芳香族磷酸酯金屬鹽之具體例,可舉出以下內容。此等可單獨包含一種,亦可包含二種以上之組合。惟,一般式(1)所表示之芳香族磷酸酯金屬鹽並非受到此等所限定者。
一般式(2)中,作為R
6~R
15所表示之碳原子數1~6之烷基,可舉出與作為R
1~R
5所表示之碳原子數1~6之烷基所例示出者相同者。
由對於成型品,賦予更優良的力學的特性之觀點來看,R
6~R
15較佳係皆為氫原子。又,由同樣的觀點來看,R
7~R
12及R
14~R
15皆為氫原子,R
6及R
13互相連結形成亞甲基、乙烷二基或2,2-丙烷二基亦佳。
M
2表示鹼金屬之情況中,作為鹼金屬,例如可舉出鋰、鈉、鉀等。此等之中,較佳為鋰、鈉,特佳為鈉。又,M
2表示鹼土類金屬之情況中,作為鹼土類金屬,例如可舉出鎂、鈣、鋇等。此等之中,鈣係特佳。
對於成型品,由賦予再更優良的力學的特性之觀點來看,p較佳為2。
作為一般式(2)所表示之脂環式二羧酸金屬鹽之具體例,例如,可舉出環己烷-1,2-二羧酸鈣、環己烷-1,2-二羧酸二鈉、雙環[2.2.1]庚烷-2,3-二羧酸鈣、雙環[2.2.1]庚烷-2,3-二羧酸二鈉等。此等可單獨包含一種,亦可包含二種以上之組合。惟,一般式(2)所表示之脂環式二羧酸金屬鹽並非受到此等所限定者。
一般式(3)中,作為R
16~R
20所表示之碳原子數1~6之烷基,可舉出與作為R
1~R
15所表示之碳原子數1~6之烷基所例示出者相同者。
一般式(3)中,作為R
17及R
18或R
19及R
20互相連結所形成之碳原子數3~6之伸烷基,可舉出例如伸丙基、伸丁基、伸戊基、伸己基等。又,作為R
17及R
18或R
19及R
20互相連結所形成之碳原子數1~4之伸烷基二氧基,可舉出例如亞甲基二氧基、伸乙基二氧基、伸丙基二氧基、伸丁基二氧基等。
作為一般式(3)中,R
17~R
20所表示之碳原子數1~6之烷氧基,可舉出例如甲氧基、乙氧基、丙氧基、n-丁氧基、異丁氧基、sec-丁氧基、tert-丁氧基、戊氧基、己氧基等。
作為一般式(3)中,R
17~R
20所表示之鹵素原子,可舉出氟原子、氯原子、溴原子、碘原子。
由對於成型品,賦予更優良的力學的特性之觀點來看,R
16~R
20各自獨立為氫原子或碳原子數1~6之烷基,且X為-CH(OH)-基係較佳。
作為一般式(3)所表示之丁二酮化合物之具體例,例如,可舉出二苯亞甲基山梨醇、雙(甲基苯亞甲基)山梨醇、雙(3,4-二甲基苯亞甲基)山梨醇、雙(p-乙基苯亞甲基)山梨醇、雙(二甲基苯亞甲基)山梨醇、1,2,3-三脫氧-4,6:5,7-o-雙(4-丙基苯亞甲基)壬醇等。
作為β晶成核劑,例如庚二酸鈣、4-環己烯-1,2-二羧酸鈣、下述一般式(4)所表示之天門冬胺酸醯胺金屬鹽等的等的羧酸金屬鹽、γ-喹吖酮、二氫喹吖酮、喹吖啶酮醌等的喹吖酮化合物、N,N’,N”-三[2-甲基環己基]-1,2,3-丙烷三羧基醯胺、N,N’-二環己基-1,4-苯二甲醯胺、N,N’,N”-三環己基-1,3,5-苯三羧基醯胺、N,N’-二環己基-2,6-萘二羧基醯胺、1,3,5-三(二甲基異丙基氨基)苯等的醯胺化合物等。
此處,一般式(4)中,M
3係表示鹼金屬、鹼土類金屬、羥基鋁或二羥基鋁,a係表示1或2,x係表示1或2,滿足ax=2。Z係表示具有下述一般式(5)或(6)所表示之構造之基。
此處,一般式(5)及(6)中,Y係表示直接鍵結或碳原子數1~4之伸烷基,R
21~R
30係分別獨立地表示氫原子、鹵素原子或碳原子數1~6之烷基,*係表示與羰基碳鍵結之位置。
一般式(4)中,作為M
3,可舉出例如鋰、鈉、鉀、鎂、鈣、鋇、羥基鋁、二羥基鋁等。由對於成型品,賦予更優良的力學的特性之觀點來看,M
3較佳為鈉、鈣、羥基鋁或二羥基鋁,較佳為鈉或羥基鋁,特佳為鈉。又,一般式(4)中,較佳係x為1、a為2。
一般式(4)中之Z較佳係具有一般式(6)所表示之構造之基。此情況中,對於成型品,可賦予更進一步優良的力學的特性。
作為一般式(5)及(6)中之Y所表示之碳原子數1~4之伸烷基,例如,可舉出亞甲基、伸乙基、伸丙基、伸丁基、伸異丁基等。由對於成型品,賦予更優良的力學的特性之觀點來看,Y較佳為直接鍵結或亞甲基,更佳為直接鍵結。
作為一般式(5)及(6)中之R
21~R
30所表示之鹵素原子,可舉出氟、氯、溴、碘。此等之中,由對於成型品,賦予更優良的力學的特性之觀點來看,特佳為氯。
作為一般式(5)及(6)中之R
21~R
30所表示之碳原子數1~6之烷基,可舉出與作為R
1~R
20所表示之碳原子數1~6之烷基所例示出者相同者。
作為一般式(5)及(6)中之R
21~R
30,由對於成型品,賦予更優良的力學的特性之觀點來看,較佳為氫原子或鹵素原子,特佳為氫原子。
作為一般式(4)所表示之天門冬胺酸醯胺金屬鹽之具體例,可舉出以下內容。此等可單獨包含一種,亦可包含二種以上之組合。惟,一般式(4)所表示之天門冬胺酸醯胺金屬鹽並非受到此等所限定者。
由賦予成型品更加優良的剛性之觀點來看,本實施形態之成核劑組成物中,較佳係包含促進聚烯烴系樹脂之α晶形成之α晶成核劑。由同樣的觀點來看,本實施形態之成核劑組成物中,較佳係包含由一般式(1)所表示之芳香族磷酸酯金屬鹽、一般式(2)所表示之脂環式二羧酸金屬鹽及芳香族羧酸金屬鹽所成之群所選出之至少一種作為α晶成核劑,更佳係包含由一般式(1)所表示之芳香族磷酸酯金屬鹽、及一般式(2)所表示之脂環式二羧酸金屬鹽所成之群所選出之至少一種。
又,由賦予成型品更加優良的耐衝撃性之觀點來看,本實施形態之成核劑組成物中,較佳係包含促進聚烯烴系樹脂之β晶形成之β晶成核劑。由同樣的觀點來看,本實施形態之成核劑組成物,較佳係包含由羧酸金屬鹽及喹吖酮化合物所成之群所選出之至少一種作為β晶成核劑,更佳係包含羧酸金屬鹽。
由賦予成型品更加優良的剛性及耐衝撃性之觀點來看,本實施形態之成核劑組成物中,較佳係包含促進聚烯烴系樹脂之α晶形成之α晶成核劑及促進聚烯烴系樹脂之β晶形成之β晶成核劑。成核劑組成物包含α晶成核劑及β晶成核劑之情況中,α晶成核劑與β晶成核劑之含有比例,例如以質量比計,為α晶成核劑/β晶成核劑=0.5/99.5~90/10即可,較佳為α晶成核劑/β晶成核劑=1/99~50/50,更佳為1.5/98.5~40/60。
本實施形態之成核劑組成物中所包含之聚烯烴系樹脂用成核劑,例如為成核劑組成物全體之10~100質量%即可,亦可為50~100質量%,亦可為80~100質量%。
此外,由賦予成型品更加優良的耐衝撃性之觀點來看,本實施形態之成核劑組成物中,較佳係不包含N,N’-二環己基-1,4-苯二甲醯胺。
本實施形態之成核劑組成物中,依需要,亦可進一步包含酚系抗氧化劑、磷系抗氧化劑、硫系抗氧化劑、其他的抗氧化劑、受阻胺化合物、紫外線吸收劑、脂肪酸金屬鹽、阻燃劑、阻燃助劑、潤滑劑、填充劑、水滑石類、靜電劑、螢光增白劑、顏料及染料等的各種添加劑。
作為酚系抗氧化劑,例如,可舉出2,6-二-tert-丁基-4-乙基苯酚、2-tert-丁基-4,6-二甲基苯酚、苯乙烯化苯酚、2,2’-亞甲基雙(4-乙基-6-tert-丁基苯酚)、2,2’-硫代雙-(6-tert-丁基-4-甲基苯酚)、2,2’-硫代二伸乙基雙[3-(3,5-二-tert-丁基-4-羥基苯基)丙酸酯]、2-甲基-4,6-雙(辛基磺醯基甲基)苯酚、2,2’-異亞丁基雙(4,6-二甲基苯酚)、異辛基-3-(3,5-二-tert-丁基-4-羥基苯基)丙酸酯、N,N’-己烷-1,6-二基雙[3-(3,5-二-tert-丁基-4-羥基苯基)丙醯胺]、2,2’-草醯胺-雙[乙基-3-(3,5-二-tert-丁基-4-羥基苯基)丙酸酯]、2-乙基己基-3-(3’,5’-二-tert-丁基-4’-羥基苯基)丙酸酯、2,2’-伸乙基雙(4,6-二-tert-丁基苯酚)、3,5-二-tert-丁基-4-羥基苯丙酸及C13-15烷基之酯、2,5-二-tert-戊基氫醌、受阻酚之聚合物(ADEKA POLYMER ADDITIVES EUROPE SAS公司製 商品名「AO.OH.98」)、2,2’-亞甲基雙[6-(1-甲基環己基)-p-甲酚]、2-tert-丁基-6-(3-tert-丁基-2-羥基5-甲基苄基)-4-甲基苯基丙烯酸酯、2-[1-(2-羥基-3,5-二-tert-戊基苯基)乙基]-4,6-二-tert-戊基苯基丙烯酸酯、6-[3-(3-tert-丁基-4-羥基-5-甲基)丙氧基]-2,4,8,10-四-tert-丁基苯并[d,f][1,3,2]-二氧雜磷、六亞甲基雙[3-(3,5-二-tert-丁基-4-羥基苯基)丙酸酯]、雙[單乙基(3,5-二-tert-丁基-4-羥基苄基)膦酸]鈣鹽、5,7-雙(1,1-二甲基乙基)-3-羥基-2(3H)-苯并呋喃酮與o-二甲苯之反應生成物、2,6-二-tert-丁基-4-(4,6-雙(辛基硫代)-1,3,5-三嗪-2-基氨基)苯酚、DL-a-生育酚(維生素E)、2,6-雙(α-甲基苄基)-4-甲基苯酚、雙[3,3-雙-(4’-羥基-3’-tert-丁基-苯基)丁酸]二醇酯、2,6-二-tert-丁基-p-甲酚、2,6-二苯基-4-十八烷基氧基苯酚、硬脂基(3,5-二-tert-丁基-4-羥基苯基)丙酸酯、二硬脂基(3,5-二-tert-丁基-4-羥基苄基)膦酸酯、十三烷基-3,5-tert-丁基-4-羥基苄基硫代乙酸酯、硫代二伸乙基雙[(3,5-二-tert-丁基-4-羥基苯基)丙酸酯]、4,4’-硫代雙(6-tert-丁基-m-甲酚)、2-辛基硫代-4,6-二(3,5-二-tert-丁基-4-羥基苯氧基)-s-三嗪、2,2’-亞甲基雙(4-甲基-6-tert-丁基苯酚)、雙[3,3-雙(4-羥基-3-tert-丁基苯基)丁酸]二醇酯、4,4’-亞丁基雙(2,6-二-tert-丁基苯酚)、4,4’-亞丁基雙(6-tert-丁基-3-甲基苯酚)、2,2’-伸乙基雙(4,6-二-tert-丁基苯酚)、1,1,3-三(2-甲基-4-羥基-5-tert-丁基苯基)丁烷、雙[2-tert-丁基-4-甲基-6-(2-羥基-3-tert-丁基-5-甲基苄基)苯基]對苯二甲酸酯、1,3,5-三(2,6-二甲基-3-羥基-4-tert-丁基苄基)異氰脲酸酯、1,3,5-三(3,5-二-tert-丁基-4-羥基苄基)異氰脲酸酯、1,3,5-三(3,5-二-tert-丁基-4-羥基苄基)-2,4,6-三甲基苯、1,3,5-三[(3,5-二-tert-丁基-4-羥基苯基)丙醯基氧基乙基]異氰脲酸酯、四[亞甲基-3-(3’,5’-tert-丁基-4’-羥基苯基)丙酸酯]甲烷、2-tert-丁基-4-甲基-6-(2-丙烯醯氧基-3-tert-丁基-5-甲基苄基)苯酚、3,9-雙[2-(3-tert-丁基-4-羥基-5-甲基氫化肉桂醯氧基)-1,1-二甲基乙基]-2,4,8,10-四氧雜螺[5.5]十一烷、三乙二醇雙[β-(3-tert-丁基-4-羥基-5-甲基苯基)丙酸酯]、硬脂基-3-(3,5-二-tert-丁基-4-羥基苯基)丙酸醯胺、棕櫚基-3-(3,5-二-tert-丁基-4-羥基苯基)丙酸醯胺、肉豆蔻基-3-(3,5-二-tert-丁基-4-羥基苯基)丙酸醯胺、月桂基-3-(3,5-二-tert-丁基-4-羥基苯基)丙酸醯胺等的3-(3,5-二烷基-4-羥基苯基)丙酸衍生物等。
作為磷系抗氧化劑,例如,可舉出三苯基亞磷酸酯、二異辛基亞磷酸酯、七(二丙二醇)三亞磷酸酯、亞磷酸三異癸酯、二苯基異辛基亞磷酸酯、二異辛基苯基亞磷酸酯、二苯基十三烷基亞磷酸酯、三異辛基亞磷酸酯、三月桂基亞磷酸酯、二苯基亞磷酸酯、三(二丙二醇)亞磷酸酯、二油基氫亞磷酸酯、三月桂基三硫代亞磷酸酯、雙(十三烷基)亞磷酸酯、三(異癸基)亞磷酸酯、三(十三烷基)亞磷酸酯、亞磷酸二苯基癸酯、二壬基苯基雙(壬基苯基)亞磷酸酯、聚(二丙二醇)苯基亞磷酸酯、四苯基二丙二醇二亞磷酸酯、三壬基苯基亞磷酸酯、三(2,4-二-tert-丁基苯基)亞磷酸酯、三(2,4-二-tert-丁基-5-甲基苯基)亞磷酸酯、三[2-tert-丁基-4-(3-tert-丁基-4-羥基-5-甲基苯基硫代)-5-甲基苯基]亞磷酸酯、三(癸基)亞磷酸酯、辛基二苯基亞磷酸酯、二(癸基)單苯基亞磷酸酯、二硬脂基季戊四醇與硬脂酸鈣鹽之混合物、烷基(C10)雙酚A亞磷酸酯、四苯基-四(十三烷基)季戊四醇四亞磷酸酯、雙(2,4-二-tert-丁基-6-甲基苯基)乙基亞磷酸酯、四(十三烷基)異亞丙基二苯酚二亞磷酸酯、四(十三烷基)-4,4’-n-亞丁基雙(2-tert-丁基-5-甲基苯酚)二亞磷酸酯、六(十三烷基)-1,1,3-三(2-甲基-4-羥基-5-tert-丁基苯基)丁烷三亞磷酸酯、四(2,4-二-tert-丁基苯基)聯苯二亞膦酸酯、9,10-二氫-9-氧雜-10-磷雜菲-10-氧化物、(1-甲基-1-丙烯基-3-亞基)三(1,1-二甲基乙基)-5-甲基-4,1-伸苯基)六-十三烷基亞磷酸酯、2,2’-亞甲基雙(4,6-二-tert-丁基苯基)-2-乙基己基亞磷酸酯、2,2’-亞甲基雙(4,6-二-tert-丁基苯基)-十八烷基亞磷酸酯、2,2’-伸乙基雙(4,6-二-tert-丁基苯基)氟亞磷酸酯、4,4’-亞丁基雙(3-甲基-6-tert-丁基苯基二-十三烷基)亞磷酸酯、三(2-[(2,4,8,10-四-tert-丁基二苯并[d,f][1,3,2]二氧磷呯(Dioxaphosphepin)-6-基)氧基]乙基)胺、3,9-雙(4-壬基苯氧基)-2,4,8,10-四氧雜-3,9-二磷雜螺[5,5]十一烷、2,4,6-三-tert-丁基苯基-2-丁基-2-乙基-1,3-丙二醇亞磷酸酯、聚4,4’-異亞丙基二苯酚C12-15醇亞磷酸酯、雙(二異癸基)季戊四醇二亞磷酸酯、雙(十三烷基)季戊四醇二亞磷酸酯、雙(十八烷基)季戊四醇二亞磷酸酯、雙(壬基苯基)季戊四醇二亞磷酸酯、雙(2,4-二-tert-丁基苯基)季戊四醇二亞磷酸酯、雙(2,4,6-三-tert-丁基苯基)季戊四醇二亞磷酸酯、雙(2,6-二-tert-丁基-4-甲基苯基)季戊四醇二亞磷酸酯、雙(2,4-二異丙苯基)季戊四醇二亞磷酸酯等。
作為硫系抗氧化劑,例如,可舉出四[亞甲基-3-(月桂基硫代)丙酸酯]甲烷、雙(甲基-4-[3-n-烷基(C12/C14)硫代丙醯基氧基]5-tert-丁基苯基)硫化物、二-十三烷基-3,3’-硫代二丙酸酯、二月桂基-3,3’-硫代二丙酸酯、二肉豆蔻基-3,3’-硫代二丙酸酯、二硬脂基-3,3’-硫代二丙酸酯、月桂基/硬脂基硫代二丙酸酯、4,4’-硫代雙(6-tert-丁基-m-甲酚)、2,2’-硫代雙(6-tert-丁基-p-甲酚)、二硬脂基-二硫醚。
作為其他的抗氧化劑,可舉出N-苄基-α-苯基硝酮、N-乙基-α-甲基硝酮、N-辛基-α-庚基硝酮、N-月桂基-α-十一烷基硝酮、N-四癸基-α-十三烷基硝酮、N-十六烷基-α-十五烷基硝酮、N-辛基-α-十七烷基硝酮、N-十六烷基-α-十七烷基硝酮、N-十八烷基-α-十五烷基硝酮、N-十七烷基-α-十七烷基硝酮、N-十八烷基-α-十七烷基硝酮等的硝酮化合物、3-芳基苯并呋喃-2(3H)-酮、3-(烷氧基苯基)苯并呋喃-2-酮、3-(醯氧基苯基)苯并呋喃-2(3H)-酮、5,7-二-tert-丁基-3-(3,4-二甲基苯基)-苯并呋喃-2(3H)-酮、5,7-二-tert-丁基-3-(4-羥基苯基)-苯并呋喃-2(3H)-酮、5,7-二-tert-丁基-3-{4-(2-羥基乙氧基)苯基}-苯并呋喃-2(3H)-酮、6-(2-(4-(5,7-二-tert-2-氧基-2,3-二氫苯并呋喃-3-基)苯氧基)乙氧基)-6-氧基己基-6-((6-羥基己醯基)氧基)己酸酯、5-二-tert-丁基-3-(4-((15-羥基-3,6,9,13-四氧雜十五烷基)氧基)苯基)苯并呋喃-2(3H)酮等的苯并呋喃化合物等。
作為受阻胺化合物,例如,可舉出2,2,6,6-四甲基-4-哌啶基硬脂酸酯、1,2,2,6,6-五甲基-4-哌啶基硬脂酸酯、2,2,6,6-四甲基-4-哌啶基苯甲酸酯、雙(2,2,6,6-四甲基-4-哌啶基)癸二酸酯、四(2,2,6,6-四甲基-4-哌啶基)-1,2,3,4-丁烷四羧酸酯、四(1,2,2,6,6-五甲基-4-哌啶基)-1,2,3,4-丁烷四羧酸酯、雙(2,2,6,6-四甲基-4-哌啶基)・二(十三烷基)-1,2,3,4-丁烷四羧酸酯、雙(1,2,2,6,6-五甲基-4-哌啶基)-二(十三烷基)-1,2,3,4-丁烷四羧酸酯、雙(1,2,2,4,4-五甲基-4-哌啶基)-2-丁基-2-(3,5-二-tert-丁基-4-羥基苄基)丙二酸酯、1-(2-羥基乙基)-2,2,6,6-四甲基-4-哌啶醇/琥珀酸二乙基聚縮合物、1,6-雙(2,2,6,6-四甲基-4-哌啶基氨基)己烷/2,4-二氯-6-嗎啉基-s-三嗪聚縮合物、1,6-雙(2,2,6,6-四甲基-4-哌啶基氨基)己烷/2,4-二氯-6-tert-辛基氨基-s-三嗪聚縮合物、1,5,8,12-四[2,4-雙(N-丁基-N-(2,2,6,6-四甲基-4-哌啶基)氨基)-s-三嗪-6-基]-1,5,8,12-四氮雜十二烷、1,5,8,12-四[2,4-雙(N-丁基-N-(1,2,2,6,6-五甲基-4-哌啶基)氨基)-s-三嗪-6-基]-1,5,8-12-四氮雜十二烷、1,6,11-三[2,4-雙(N-丁基-N-(2,2,6,6-四甲基-4-哌啶基)氨基)-s-三嗪-6-基氨基]十一烷、1,6,11-三[2,4-雙(N-丁基-N-(1,2,2,6,6-五甲基-4-哌啶基)氨基)-s-三嗪-6-基氨基]十一烷、3,9-雙[1,1-二甲基-2-{三(2,2,6,6-四甲基-4-哌啶基氧基羰基)丁基羰基氧基}乙基]-2,4,8,10-四氧雜螺[5.5]十一烷、3,9-雙[1,1-二甲基-2-{三(1,2,2,6,6-五甲基-4-哌啶基氧基羰基)丁基羰基氧基}乙基]-2,4,8,10-四氧雜螺[5.5]十一烷、雙(1-十一烷基氧基-2,2,6,6-四甲基哌啶-4-基)碳酸酯、2,2,6,6-四甲基-4-十六烷酸哌啶酯、2,2,6,6-四甲基-4-哌啶基十八酸酯等。
作為紫外線吸收劑,例如,可舉出2,4-二羥基二苯甲酮、5,5’-亞甲基雙(2-羥基-4-甲氧基二苯甲酮)等的2-羥基二苯甲酮類;2-(2-羥基-5-甲基苯基)苯并三唑、2-(2-羥基-5-tert-辛基苯基)苯并三唑、2-(2-羥基-3,5-二-tert-丁基苯基)-5-氯苯并三唑、2-(2-羥基-3-tert-丁基-5-甲基苯基)-5-氯苯并三唑、2-(2-羥基-3,5-二異丙苯基)苯并三唑、2,2’-亞甲基雙(4-tert-辛基-6-苯并三唑基苯酚)、2-(2-羥基-3-tert-丁基-5-羧基苯基)苯并三唑之聚乙二醇酯、2-[2-羥基-3-(2-丙烯醯氧基乙基)-5-甲基苯基]苯并三唑、2-[2-羥基-3-(2-甲基丙烯醯氧基乙基)-5-tert-丁基苯基]苯并三唑、2-[2-羥基-3-(2-甲基丙烯醯氧基乙基)-5-tert-辛基苯基]苯并三唑、2-[2-羥基-3-(2-甲基丙烯醯氧基乙基)-5-tert-丁基苯基]-5-氯苯并三唑、2-[2-羥基-5-(2-甲基丙烯醯氧基乙基)苯基]苯并三唑、2-[2-羥基-3-tert-丁基-5-(2-甲基丙烯醯氧基乙基)苯基]苯并三唑、2-[2-羥基-3-tert-戊基-5-(2-甲基丙烯醯氧基乙基)苯基]苯并三唑、2--[2-羥基-3-tert-丁基-5-(3-甲基丙烯醯氧基丙基)苯基]-5-氯苯并三唑、2--[2-羥基-4-(2-甲基丙烯醯氧基甲基)苯基]苯并三唑、2--[2-羥基-4-(3-甲基丙烯醯氧基-2-羥基丙基)苯基]苯并三唑、2--[2-羥基-4-(3-甲基丙烯醯氧基丙基)苯基]苯并三唑等的2-(2-羥基苯基)苯并三唑類;苯基水楊酸酯、間苯二酚單苯甲酸酯、2,4-二-tert-丁基苯基-3,5-二-tert-丁基-4-羥基苯甲酸酯、辛基(3,5-二-tert-丁基-4-羥基)苯甲酸酯、十二基(3,5-二-tert-丁基-4-羥基)苯甲酸酯、四癸基(3,5-二-tert-丁基-4-羥基)苯甲酸酯、十六烷基(3,5-二-tert-丁基-4-羥基)苯甲酸酯、十八烷基(3,5-二-tert-丁基-4-羥基)苯甲酸酯、二十二基(3,5-二-tert-丁基-4-羥基)苯甲酸酯等的苯甲酸酯類;2-乙基-2’-乙氧基草醯替苯胺、2-乙氧基-4’-十二基草醯替苯胺等的取代草醯替苯胺類;乙基-α-氰基-β,β-二苯基丙烯酸酯、甲基-2-氰基-3-甲基-3-(p-甲氧基苯基)丙烯酸酯等的氰基丙烯酸酯類;2-(4,6-二苯基-1,3,5-三嗪-2-基)-5-己基氧基苯酚、2-(2-羥基-4-辛氧基苯基)-4,6-雙(2,4-二甲基苯基)-1,3,5-三嗪、三辛基-2,2’,2”-((1,3,5-三嗪-2,4,6-三基)三(3-羥基苯-4-,1-二基)三丙酸酯)、2-(4,6-二苯基-1,3,5-三嗪-2-基)-5-[2-(2-乙基己醯基氧基)乙氧基]苯酚、2,4,6-三(2-羥基-4-己基氧基-3-甲基苯基)-1,3,5-三嗪、1,12-雙[2-[4-(4,6-二苯基-1,3,5-三嗪-2-基)-3-羥基苯氧基]乙基]十二烷二酸酯等的三嗪類;各種之金屬鹽,或金屬螯合物,尤其,可舉出鎳、鉻之鹽,或螯合物類等。
作為脂肪酸金屬鹽,例如,可舉出包含直鏈或分支狀之脂肪酸殘基之碳原子數12~20之脂肪酸之金屬鹽等。作為構成脂肪酸金屬鹽之金屬離子,例如,可舉出鈉離子、鉀離子、鋰離子、二羥基鋁離子、鈣離子、鋅離子、鋇離子、鎂離子、羥基鋁離子等,此等之中,特佳為鈉離子、鉀離子、鋰離子、鈣離子。
作為脂肪酸金屬鹽之具體例,可舉出月桂酸鈉、肉豆蔻酸鈉、棕櫚酸鈉、硬脂酸鈉、油酸鈉、亞油酸鈉、亞麻酸鈉、花生酸鈉、12-羥基硬脂酸鈉、月桂酸鉀、肉豆蔻酸鉀、棕櫚酸鉀、硬脂酸鉀、油酸鉀、亞油酸鉀、亞麻酸鉀、花生酸鉀、12-羥基硬脂酸鉀、月桂酸鋰、肉豆蔻酸鋰、棕櫚酸鋰、硬脂酸鋰、油酸鋰、亞油酸鋰、亞麻酸鋰、花生酸鋰、12-羥基硬脂酸鋰、月桂酸鈣、肉豆蔻酸鈣、棕櫚酸鈣、硬脂酸鈣、油酸鈣、亞油酸鈣、亞麻酸鈣、花生酸鈣、12-羥基硬脂酸鈣等,此等之中,較佳為肉豆蔻酸鈉、硬脂酸鈉、12-羥基硬脂酸鈉、肉豆蔻酸鋰、硬脂酸鋰、12-羥基硬脂酸鋰、肉豆蔻酸鈣、硬脂酸鈣、12-羥基硬脂酸鈣,更佳為肉豆蔻酸鋰、硬脂酸鋰、12-羥基硬脂酸鋰、肉豆蔻酸鈣、硬脂酸鈣、12-羥基硬脂酸鈣,再更佳為肉豆蔻酸鋰、硬脂酸鋰、12-羥基硬脂酸鋰。
作為阻燃劑,例如,可舉出磷酸三苯酯、磷酸三甲苯酯、磷酸三二甲苯酯、甲苯基二苯基磷酸酯、甲苯基-2,6-二甲苯基磷酸酯、間苯二酚雙(二苯基磷酸酯)、(1-甲基伸乙基)-4,1-伸苯基四苯基二磷酸酯、1,3-伸苯基四(2,6-二甲基苯基)磷酸酯、ADEKA股份公司製之商品名「Adekastab FP-500」、「Adekastab FP-600」、
「Adekastab FP-800」之芳香族磷酸酯、苯基膦酸二乙烯酯、苯基膦酸二烯丙酯、苯基膦酸(1-丁烯基)等的膦酸酯、二苯基次膦酸苯酯、二苯基次膦酸甲酯、9,10-二氫-9-氧雜-10-磷雜菲-10-氧化物衍生物等的次膦酸酯、雙(2-烯丙基苯氧基)磷腈、二甲苯基磷腈等的磷腈化合物、磷酸三聚氰胺、焦磷酸三聚氰胺、多磷酸三聚氰胺、多磷酸蜜白胺、多磷酸銨、磷酸哌𠯤、焦磷酸哌𠯤、多磷酸哌𠯤、含有磷之乙烯基苄基化合物及紅磷等的磷系阻燃劑、氫氧化鎂、氫氧化鋁等的金屬氫氧化物、溴化雙酚A型環氧樹脂、溴化苯酚酚醛清漆型環氧樹脂、六溴苯、五溴甲苯、伸乙基雙(五溴苯基)、伸乙基雙四溴鄰苯二甲醯亞胺、1,2-二溴-4-(1,2-二溴乙基)環己烷、四溴環辛烷、六溴環十二烷、雙(三溴苯氧基)乙烷、溴化聚苯基醚、溴化聚苯乙烯及2,4,6-三(三溴苯氧基)-1,3,5-三嗪、三溴苯基馬來醯亞胺、三溴苯基丙烯酸酯、三溴苯基甲基丙烯酸酯、四溴雙酚A型二甲基丙烯酸酯、五溴苄基丙烯酸酯,及,溴化苯乙烯等的溴系阻燃劑等。此等阻燃劑較佳為與氟樹脂等的抗滴落劑或多元醇、水滑石等的阻燃助劑併用。
作為潤滑劑,例如,可舉出油酸醯胺、芥酸醯胺等的不飽和脂肪酸醯胺;二十二酸醯胺、硬脂酸醯胺等的飽和脂肪酸醯胺、丁基硬脂酸酯、硬脂基醇、硬脂酸單甘油酯、山梨醇酐單棕櫚酸酯、山梨醇酐單硬脂酸酯、甘露糖醇、硬脂酸、硬化蓖麻油、硬脂酸醯胺、油酸醯胺、伸乙基雙硬脂酸醯胺等。
作為填充劑,例如可舉出滑石、雲母、碳酸鈣、酸化鈣、氫氧化鈣、碳酸鎂、氫氧化鎂、酸化鎂、硫酸鎂、氫氧化鋁、硫酸鋇、玻璃粉末、玻璃纖維、黏土、白雲石、二氧化矽、氧化鋁、鈦酸鉀晶鬚、矽灰石、纖維狀硫酸氧化鎂等,可適宜選擇粒子徑(於纖維狀時為纖維徑或纖維長及縱橫比)使用。此等填充劑之中,由於賦予剛性之效果優良、且入手容易,故特佳係使用滑石。又,填充劑視需要可使用經表面處理者。
水滑石類,可舉出作為天然物或合成物所知之包含鎂、鋁、羥基、碳酸基及任意結晶水之複合鹽化合物、鎂或鋁之一部份經鹼金屬或鋅等其他金屬取代而成者,或羥基、碳酸基經其他陰離子基取代而成者。水滑石類可為使結晶水脫水而成者,亦可為經硬脂酸等的高級脂肪酸、油酸鹼金屬鹽等的高級脂肪酸金屬鹽、十二烷基苯磺酸鹼金屬鹽等的有機磺酸金屬鹽、高級脂肪酸醯胺、高級脂肪酸酯或蠟等被覆者。水滑石類可為天然物,又,亦可為合成品。作為水滑石類之合成方法,可舉出日本特公昭46-2280號公報、日本特公昭50-30039號公報、日本特公昭51-29129號公報、日本特公平3-36839號公報、日本特開昭61-174270號公報、日本特開平5-179052號公報等中所記載之公知的方法。又,水滑石類係可不受其結晶構造、結晶粒子等限制而使用。
作為靜電劑,例如,可舉出藉由非離子性、陰離子性、陽離子性或兩性的界面活性劑等所產生之低分子型靜電劑、藉由高分子化合物所產生之高分子型靜電劑。作為非離子性界面活性劑,可舉出高級醇環氧乙烷附加物、脂肪酸環氧乙烷附加物、高級烷基胺環氧乙烷附加物、聚烯烴二醇環氧乙烷附加物等的聚乙二醇型非離子界面活性劑;聚乙烯氧化物、丙三醇之脂肪酸酯、季戊四醇之脂肪酸酯、山梨糖醇或者山梨醇酐之脂肪酸酯、多元醇之烷基醚、烷醇胺之脂肪族醯胺等的多元醇型非離子界面活性劑等,作為陰離子性界面活性劑,例如,可舉出高級脂肪酸之鹼金屬鹽等的羧酸鹽;高級醇硫酸酯鹽、高級烷基醚硫酸酯鹽等的硫酸酯鹽、烷基苯磺酸鹽、烷基磺酸鹽、石蠟磺酸鹽等的磺酸鹽;高級醇磷酸酯鹽等的磷酸酯鹽等,作為陽離子性界面活性劑,可舉出烷基三甲基銨鹽等的第4級銨鹽等。作為兩性界面活性劑,可舉出高級烷基氨基丙酸鹽等的氨基酸型兩性界面活性劑、高級烷基二甲基甜菜鹼、高級烷基二羥基乙基甜菜鹼等的甜菜鹼型兩性界面活性劑等。此等之中,較佳為陰離子性界面活性劑,特佳為烷基苯磺酸鹽、烷基磺酸鹽、石蠟磺酸鹽等的磺酸鹽。
作為高分子型靜電劑,可舉出離子聚合物或將聚乙二醇作為親水部之嵌段聚合物等。作為離子聚合物,可舉出日本特開2010-132927號公報中所記載之離子聚合物。作為將聚乙二醇作為親水部之聚合物,例如,可舉出日本特開平7-10989號公報中記載之聚醚酯醯胺、美國專利第6552131號公報記載之聚烯烴與聚乙二醇所構成之聚合物、日本特開2016-023254號公報記載之聚酯與聚乙二醇所構成之聚合物等。
所謂螢光增白劑,係指藉由吸收太陽光或人工光之紫外線,並將其轉變為紫~青色之可視光線而輻射之螢光作用,來助長成型體之白色度或藍色調之化合物。作為螢光增白劑,可舉出苯并噁唑系化合物C.I. Fluorescent Brightener184;香豆素系化合物C.I. Fluorescent Brightener52;二氨基茋二磺酸酸系化合物C.I. Fluorescent Brightener24、85、71等。
作為顏料,並非受到特別限定者,亦可使用市售的顏料。作為顏料之具體例,例如,可舉出色素紅1、2、3、9、10、17、22、23、31、38、41、48、49、88、90、97、112、119、122、123、144、149、166、168、169、170、171、177、179、180、184、185、192、200、202、209、215、216、217、220、223、224、226、227、228、240、254;色素橘13、31、34、36、38、43、46、48、49、51、52、55、59、60、61、62、64、65、71;色素黃1、3、12、13、14、16、17、20、24、55、60、73、81、83、86、93、95、97、98、100、109、110、113、114、117、120、125、126、127、129、137、138、139、147、148、150、151、152、153、154、166、168、175、180、185;色素綠7、10、36;色素藍15、15:1、15:2、15:3、15:4、15:5、15:6、22、24、29、56、60、61、62、64;色素紫1、15、19、23、27、29、30、32、37、40、50等。
作為染料,可舉出偶氮染料、蒽醌染料、靛藍染料、三芳基甲烷染料、氧雜蒽染料、茜素染料、吖啶染料、茋染料、噻唑染料、萘酚染料、喹啉染料、硝基染料、吲達胺染料、㗁𠯤染料、酞菁染料、花青染料等。
本實施形態之成核劑組成物亦可為進一步摻合黏合劑、蠟、溶劑、二氧化矽等的造粒助劑,並經造粒之單包複合添加劑。又,本實施形態之成核劑組成物亦可為進一步包含聚烯烴系樹脂之母料。
作為母料中所包含之聚烯烴系樹脂,例如,可舉出低密度聚乙烯、直鏈狀低密度聚乙烯、高密度聚乙烯、交聯聚乙烯、超高分子量聚乙烯等的聚乙烯系樹脂、均聚聚丙烯、隨機共聚物聚丙烯、嵌段共聚物聚丙烯、衝擊共聚物聚丙烯、高衝擊共聚物聚丙烯、馬來酸酐改質聚丙烯等的聚丙烯系樹脂、聚丁烯-1、環烯烴聚合物、聚-3-甲基-1-丁烯、聚-3-甲基-1-戊烯、聚-4-甲基-1-戊烯等的α-烯烴聚合物、伸乙基-甲基甲基丙烯酸酯共聚合物、伸乙基-乙酸乙烯酯共聚合物等的α-烯烴共聚合物等。此等聚烯烴系樹脂係可單獨使用1種,亦可併用2種以上。又,聚烯烴系樹脂亦可經合金化。聚烯烴系樹脂之分子量、聚合度、密度、軟化點、對於溶媒之不溶分之比例、立體規則性之程度、觸媒殘渣之有無、原料之單體之種類或摻合比率、聚合中所使用之觸媒之種類(例如、齊格勒觸媒、茂金屬觸媒等)等並非特別限定者,係可適宜選擇。
作為母料中所包含之聚烯烴系樹脂,聚丙烯系樹脂係特佳。
成核劑組成物為包含聚烯烴系樹脂之母料之情況中,母料中之聚烯烴系樹脂之含量,例如,90質量%以下即可,較佳為80質量%以下,更佳為60質量%以下。又,母料中之聚烯烴系樹脂之含量,例如,為20質量%以上即可。
接著,針對本實施形態之樹脂組成物進行說明。
<樹脂組成物>
本實施形態之樹脂組成物係包含聚烯烴系樹脂,及至少一種聚烯烴系樹脂用成核劑,且藉由以下之方法所算出之β晶分率為0.2~71%。
<β晶分率之算出方法>
(1)在使樹脂組成物於80℃下乾燥8小時後,由乾燥後之團塊取樣出10mg之試料,導入示差掃描熱量測定裝置中。
(2)使用示差掃描熱量測定裝置,將試料以自25℃起以50℃/min之速度昇溫至230℃為止,於230℃下保持20分鐘後,以100℃/min之速度冷卻至50℃為止,於50℃下保持20分鐘後,以30℃/min之速度昇溫至230℃為止之溫度程序來進行示差掃描熱量測定,並將橫軸設為溫度θ(℃)、縱軸設為熱流量Q(mW),獲得DSC曲線Q=f(θ)。此處,針對縱軸,係將吸熱設為正的方向。
(3)於DSC曲線之對應於上述溫度程序中之第2次之昇溫過程之部分中,由f(θ)將基準線g(θ)=(f(200)-f(110))/90×(θ-110)+f(110)扣除,獲得經基準線補正之DSC曲線Q’=h(θ)=f(θ)-g(θ)。
(4)將由曲線Q’=h(θ)之110≦θ≦200之部分及連結點A(110,0)及點B(200,0)之線段AB所包圍之領域之面積設為S
t。此處,S
t係以下述公式表示。
(5)將曲線Q’=h(θ)上之110≦θ≦200之範圍中之2個極大點設為R(θ
β,h(θ
β)),S(θ
α,h(θ
α))(惟θ
β<θ
α),並將曲線Q’=h(θ)上之θ
β<θ<θ
α之範圍中之極小點設為C(θ
γ,h(θ
γ)。然後,通過點C,拉出與曲線Q’=h(θ)在110<θ<θ
β之範圍內相接觸之切線,並將接點設為點D(θ
δ,h(θ
δ)。然後,係將由曲線Q’=h(θ)之θ
δ≦θ≦θ
γ之部分及連結點D及點C之線段DC所包圍之領域之面積設為S
β。
此處,S
β係以下述公式表示。
惟,j(θ)=h(θ)-i(θ),i(θ)=(h(θ
γ)-h(θ
δ))/(θ
γ-θ
δ)×(θ-θ
γ)+ h(θ
γ)。
(6)由S
t及S
β,藉由下述公式來算出β晶分率(%)。
β晶分率=S
β/S
t×100(%)
如同上述,β晶分率(%)係意指相對於被110℃~200℃之範圍中之曲線Q’與線段AB包圍之領域面積S
t,被曲線Q’與線段CD包圍之領域面積S
β之比例(參照圖2)。
依據本實施形態之樹脂組成物,可賦予包含聚烯烴系樹脂之成型品優良的力學的特性。
如同上述,本實施形態之樹脂組成物之β晶分率為0.2~71%。由賦予成型品更加優良的力學的特性之觀點來看,實施形態之樹脂組成物之β晶分率較佳為0.3~70.0%,更佳為3.0~45.0%,再更佳為5.0~30.0%,又再進一步更佳為10.0~25.0%。
作為本實施形態之樹脂組成物中所包含之聚烯烴系樹脂,可舉出與上述母料中所包含之聚烯烴系樹脂相同者。作為樹脂組成物中所包含之聚烯烴樹脂,此等之中,較佳為聚丙烯系樹脂。此情況中,將樹脂組成物成型所獲得之成型品係成為在具備優良的力學的特性的同時,亦具備優良的耐熱性者。
又,作為本實施形態之樹脂組成物中所包含之聚烯烴系樹脂用成核劑,可舉出與上述之成核劑組成物中所包含之聚烯烴系樹脂用成核劑相同者。
此外,由賦予成型品更加優良的耐衝撃性之觀點來看,本實施形態之樹脂組成物較佳係不包含N,N’-二環己基-1,4-苯二甲醯胺。
聚烯烴系樹脂用成核劑相對於聚烯烴系樹脂100質量份之含量,係未受到特別限定,例如為0.001~10質量份即可。由使樹脂組成物成型所獲得之成型品成為力學的特性更優良者,且,由充分地抑制由成型品產生之起霜或聚烯烴系樹脂用成核劑之轉移之觀點來看,聚烯烴系樹脂用成核劑相對於聚烯烴系樹脂100質量份之含量,較佳為0.01~1質量份,更佳為0.02~0.2質量份。
本實施形態之樹脂組成物中,依需要,亦可進一步包含酚系抗氧化劑、磷系抗氧化劑、硫系抗氧化劑、其他的抗氧化劑、受阻胺化合物、紫外線吸收劑、脂肪酸金屬鹽、阻燃劑、阻燃助劑、潤滑劑、填充劑、水滑石類、靜電劑、螢光增白劑、顏料及染料等的各種添加劑。此等各種添加劑,可舉出與作為可包含於上述之成核劑組成物之各種添加劑所舉出者相同者。
接著,係針對本實施形態之樹脂組成物之製造方法進行說明。
<樹脂組成物之製造方法>
本實施形態之樹脂組成物之製造方法係包含將至少一種聚烯烴系樹脂用成核劑,以使藉由以下之方法所算出之β晶分率成為0.2~71%的方式,摻合於聚烯烴系樹脂中之摻合步驟。由賦予成型品更加優良的力學的特性之觀點來看,較佳係以使β晶分率成為0.3~70.0%的方式進行摻合,更佳係以使其成為3.0~45.0%的方式進行摻合,再更佳係以使其成為5.0~30.0%的方式進行摻合,再進一步更佳係以使其成為10.0~25.0%的方式進行摻合。
<β晶分率之算出方法>
(1)在使樹脂組成物於80℃下乾燥8小時後,由乾燥後之團塊取樣出10mg之試料,導入示差掃描熱量測定裝置中。
(2)使用示差掃描熱量測定裝置,將試料以自25℃起以50℃/min之速度昇溫至230℃為止,於230℃下保持20分鐘後,以100℃/min之速度冷卻至50℃為止,於50℃下保持20分鐘後,以30℃/min之速度昇溫至230℃為止之溫度程序來進行示差掃描熱量測定,並將橫軸設為溫度θ(℃)、縱軸設為熱流量Q(mW),獲得DSC曲線Q=f(θ)。此處,針對縱軸,係將吸熱設為正的方向。
(3)由DSC曲線之對應於溫度程序中之第2次之昇溫過程之部分中,由f(θ)將基準線g(θ)=(f(200)-f(110))/90×(θ-110)+f(110)扣除,獲得經基準線補正之DSC曲線Q’=h(θ)=f(θ)-g(θ)。
(4)將由曲線Q’=h(θ)之110≦θ≦200之部分及連結點A(110,0)及點B(200,0)之線段AB所包圍之領域之面積設為S
t。此處,S
t係以下述公式表示。
(5)將曲線Q’=h(θ)上之110≦θ≦200之範圍中之2個極大點設為R(θ
β,h(θ
β)),S(θ
α,h(θ
α))(惟θ
β<θ
α),並將曲線Q’=h(θ)上之θ
β<θ<θ
α之範圍中之極小點設為C(θ
γ,h(θ
γ)。然後,通過點C,拉出與曲線Q’=h(θ)在110<θ<θ
β之範圍內相接觸之切線,並將接點設為點D(θ
δ,h(θ
δ)。然後,係將由曲線Q’=h(θ)之θ
δ≦θ≦θ
γ之部分及連結點D及點C之線段DC所包圍之領域之面積設為S
β。
此處,S
β係以下述公式表示。
惟,j(θ)=h(θ)-i(θ),i(θ)=(h(θ
γ)-h(θ
δ))/(θ
γ-θ
δ)×(θ-θ
γ)+ h(θ
γ)。
(6)由S
t及S
β,藉由下述公式來算出β晶分率(%)。
β晶分率=S
β/S
t×100(%)
如同上述,β晶分率(%)係意指相對於被110℃~200℃之範圍中之曲線Q’與線段AB包圍之領域面積S
t,被曲線Q’與線段CD包圍之領域面積S
β之比例(參照圖2)。
依據本實施形態之樹脂組成物之製造方法,可製造可賦予包含聚烯烴系樹脂之成型品優良的力學的特性樹脂組成物。
(準備步驟)
本實施形態之製造方法中,首先,係準備上述之聚烯烴系樹脂,及上述之成核劑組成物。
(摻合步驟)
接著,將成核劑組成物摻合於聚烯烴系樹脂中。作為摻合之方法,並非特別限定者,例如,可舉出在添加聚烯烴系樹脂、成核劑組成物,及,依需要之上述之各種添加劑後,使用FM混合機、軋輥、班布里混合機、超級混合機等的混合裝置進行混合之方法等。此處,成核劑組成物之構成成分及上述之各種添加劑中之至少一個成分亦可於聚烯烴系樹脂單體或寡聚物之聚合前或聚合中添加,並於所獲得之聚合物中添加剩下的成分。
藉由上述之方式來進行,製造樹脂組成物。樹脂組成物亦可以包含將上述之成核劑組成物中所包含之聚烯烴系樹脂用成核劑各自摻合於聚烯烴系樹脂中之步驟之方法來製造。又,樹脂組成物之製造方法亦可為包含將藉由上述之方法所獲得之混合物進一步使用單軸擠壓機或雙軸擠壓機等的熔融混練裝置進行熔融混練之熔融混練步驟之方法。此處,熔融混練之溫度,例如,為160~260℃即可。又,樹脂組成物之製造方法,亦可為包含將藉由熔融混練所獲得之混練物進行造粒之造粒步驟之方法。此處,作為造粒之方法,並非特別限定者,可舉出例如使用造粒機等的造粒裝置之方法等。進行造粒所獲得之樹脂組成物之形狀係未受到特別限定,例如,為團塊狀即可。
接著,係針對本實施形態之成型品進行說明。
<成型品>
本實施形態之成型品係將上述之樹脂組成物成型所獲得者。此成型品係具備優良的力學的特性者。
作為本實施形態之成型品,例如,可舉出射出成型品、纖維、扁紗、雙軸延伸薄膜、單軸延伸薄膜、無延伸薄膜、薄片、熱壓成型成型品、擠出吹塑成型品、射出吹塑成型品、射出延伸吹塑成型品、異型擠出(Profile Extrusion) 成型品、旋轉成型品等,更進一步具體而言,汽車外裝零件、汽車內裝零件、殼體、容器、配管等。作為汽車外裝零件,例如,可舉出保險桿、散熱器格柵、前面進氣格柵、前面板、擋泥板、柱、柱蓋、車門後視鏡撐蓋、玻璃導槽、後視鏡外殼、燈罩外殼、輪蓋、擾流板、空氣擾流板、擋風雨條、窗口壓條(Window molding)、皮帶壓條(Belt molding)、天窗、前端模塊(front-endmodule)、車門模塊、後車門模塊、外殼等,作為汽車內裝零件,例如,可舉出儀錶板、門內飾板、立柱飾板、門飾板、支柱裝飾件、整裝式塔盤、後托盤、控制台盒、空調管道等,作為殼體,例如,可舉出家電用殼體、街機遊戲機用殼體、家庭用遊戲機用殼體、攜帶型遊戲機用殼體、相機用殼體、手機用殼體、智慧型手機用殼體、電子機器用殼體、二次電池用殼體、安全斷路器用殼體等,作為容器,例如,可舉出餐具、熟食容器、冷凍食品容器、微波爐耐熱容器、冷凍保存容器、蒸煮容器、杯子、冷凍甜點杯等的食品用容器、飲料瓶、輸液瓶、醫療用中空瓶等的瓶容器、燒杯、量筒等的理化學試驗用容器、藥品容器、醫療用容器、洗劑容器、化粧品容器、香水容器、碳粉容器等,作為配管,例如,可舉出自來水管、瓦斯管、基礎設施用管、工廠公用事業用管、車輛用燃油輸送管、車輛用進氣管等的各種管、化粧品・香水噴霧用管、醫療用管、輸液管等的各種管、水管軟管、車輛用風管軟管等的各種軟管等。
作為本實施形態之成型品之成型方法,並非特別限定者,例如,可舉出射出成型法、擠出成型法、吹塑成型法、旋轉成型、真空成型法、充氣成型法、軋光成型法、搪塑成型法、浸漬成型法、熱壓成型成型法等。
[實施例]
以下,針對本發明利用實施例進一步詳細地說明,然而本發明並非受到此等所限定者。
<成核劑組成物之調製>
將下述之聚烯烴系樹脂用成核劑以表1~4所示之摻合比例摻合,並使用FM混合機(FM-20型,Nippon Coke股份公司製),於40℃下混合20分鐘,藉此獲得成核劑組成物。此外,表1~4中,成核劑之摻合比例之單位為質量%。
成核劑-1:鈉 2,2’-亞甲基雙(4,6-二-tert-丁基苯基)磷酸酯
成核劑-2:環己烷-1,2-二羧酸鈣
成核劑-3:安息香酸鈉
成核劑-4:庚二酸鈣
成核劑-5:4-環己烯-1,2-二羧酸鈣
成核劑-6:γ-喹吖酮
成核劑-7:N-苯甲醯基-L-天門冬胺酸二鈉
<β晶分率之算出>
針對藉由上述之方式所獲得之成核劑組成物,藉由下述之方法,算出β晶分率。
(1)依據JIS K 7210,摻合以溫度230℃、荷重2.16kg之條件所測定出之熔體流動速率為8g/10分之均聚聚丙烯100質量份、成核劑組成物0.10質量份、四[亞甲基-3-(3’,5’-tert-丁基-4’-羥基苯基)丙酸酯]甲烷0.05質量份、三(2,4-二-tert-丁基苯基)亞磷酸酯)0.1質量份及硬脂酸鈣0.05質量份,並使用FM混合機(FM-20型,Nippon Coke股份公司製),於40℃下混合1分鐘,獲得樹脂摻合物。
(2)使用雙軸擠壓機(東洋精機製作所製 Labo
Plastomill Micro),將樹脂摻合物於熔融溫度230℃下進行熔融混練,並將所獲得之熔融混練物進行造粒,獲得團塊。
(3)使團塊於80℃下乾燥8小時後,由乾燥後之團塊取樣出10mg之試料,導入示差掃描熱量測定裝置(Perkinelmer公司製 Diamond)中。
(4)使用示差掃描熱量測定裝置,將試料以自25℃起以50℃/min之速度昇溫至230℃為止,於230℃下保持20分鐘後,以100℃/min之速度冷卻至50℃為止,於50℃下保持20分鐘後,以30℃/min之速度昇溫至230℃為止之溫度程序來進行示差掃描熱量測定,並將橫軸設為溫度θ(℃)、縱軸設為熱流量Q(mW),獲得DSC曲線Q=f(θ)。此處,關於縱軸,係將吸熱設為正的方向。
(5)於DSC曲線之對應於上述溫度程序中之第2次之昇溫過程之部分中,由f(θ)將基準線g(θ)=(f(200)-f(110))/90×(θ-110)+f(110)扣除,獲得經基準線補正之DSC曲線Q’=h(θ)=f(θ)-g(θ)。
(6)將由曲線Q’=h(θ)之110≦θ≦200之部分及連結點A(110,0)及點B(200,0)之線段AB所包圍之領域之面積設為S
t。此處,S
t係以下述公式表示。
(7)將曲線Q’=h(θ)上之110≦θ≦200之範圍中之2個極大點設為R(θ
β,h(θ
β)),S(θ
α,h(θ
α))(惟θ
β<θ
α),並將曲線Q’=h(θ)上之θ
β<θ<θ
α之範圍中之極小點設為C(θ
γ,h(θ
γ)。然後,通過點C,拉出與曲線Q’=h(θ)在110<θ<θ
β之範圍內相接觸之切線,並將接點設為點D(θ
δ,h(θ
δ)。然後,將由曲線Q’=h(θ)之θ
δ≦θ≦θ
γ之部分及連結點D及點C之線段DC所包圍之領域之面積設為S
β。
此處,S
β係以下述公式表示。
惟,j(θ)=h(θ)-i(θ),i(θ)=(h(θ
γ)-h(θ
δ))/(θ
γ-θ
δ)×(θ-θ
γ)+ h(θ
γ)。
(8)由S
t及S
β,藉由下述公式算出β晶分率(%)。
β晶分率=S
β/S
t×100(%)
結果併記於表1~4中。
<樹脂組成物之調製>
(實施例1~13、比較例1~10)
對於聚烯烴系樹脂(依據JIS K 7210,以溫度230℃、荷重2.16kg之條件所測定出之熔體流動速率為8g/10min之均聚聚丙烯)100質量份,摻合四[亞甲基-3-(3’,5’-二-tert-丁基-4’-羥基苯基)丙酸酯]甲烷0.05質量份作為酚系抗氧化劑、三(2,4-二-tert-丁基苯基)亞磷酸酯0.1質量份作為磷系抗氧化劑、硬脂酸鈣0.05質量份作為脂肪酸金屬鹽,以及,將表5~9所示之成核劑組成物以同表中所示之摻合量進行摻合,使用FM混合機(FM-20型,Nippon Coke股份公司製),於40℃下混合1分鐘後,使用雙軸擠壓機(東洋精機製作所製 Labo Plastomill Micro),於熔融溫度230℃下進行熔融混練,並進行造粒,獲得樹脂組成物之團塊。此外。表5~9中,樹脂組成物之摻合量及樹脂組成物中之成核劑之含量之單位為質量份。
<β晶分率之算出>
針對藉由上述之方式所獲得之樹脂組成物,藉由下述之方法,算出β晶分率。
(1)在使樹脂組成物於80℃下乾燥8小時後,由乾燥後之團塊取樣出10mg之試料,導入示差掃描熱量測定裝置(Perkinelmer公司製 Diamond)中。
(2)使用示差掃描熱量測定裝置,將試料以自25℃起以50℃/min之速度昇溫至230℃為止,於230℃下保持20分鐘後,以100℃/min之速度冷卻至50℃為止,於50℃下保持20分鐘後,以30℃/min之速度昇溫至230℃為止之溫度程序來進行示差掃描熱量測定,並將橫軸設為溫度θ(℃)、縱軸設為熱流量Q(mW),獲得DSC曲線Q=f(θ)。此處,關於縱軸,係將吸熱設為正的方向。
(3)於DSC曲線之對應於上述溫度程序中之第2次之昇溫過程之部分中,由f(θ)將基準線g(θ)=(f(200)-f(110))/90×(θ-110)+f(110)扣除,獲得經基準線補正之DSC曲線Q’=h(θ)=f(θ)-g(θ)。
(4)將由曲線Q’=h(θ)之110≦θ≦200之部分及連結點A(110,0)及點B(200,0)之線段AB所包圍之領域之面積設為S
t。此處,S
t係以下述公式表示。
(5)將曲線Q’=h(θ)上之110≦θ≦200之範圍中之2個極大點設為R(θ
β,h(θ
β)),S(θ
α,h(θ
α))(惟θ
β<θ
α),並將曲線Q’=h(θ)上之θ
β<θ<θ
α之範圍中之極小點設為C(θ
γ,h(θ
γ)。然後,通過點C,拉出與曲線Q’=h(θ)在110<θ<θ
β之範圍內相接觸之切線,並將接點設為點D(θ
δ,h(θ
δ)。然後,將由曲線Q’=h(θ)之θ
δ≦θ≦θ
γ之部分及連結點D及點C之線段DC所包圍之領域之面積設為S
β。
此處,S
β係以下述公式表示。
惟,j(θ)=h(θ)-i(θ),i(θ)=(h(θ
γ)-h(θ
δ))/(θ
γ-θ
δ)×(θ-θ
γ)+ h(θ
γ)。
(6)由S
t及S
β,藉由下述公式算出β晶分率(%)。
β晶分率=S
β/S
t×100(%)
結果併記於表5~9。
此外,圖1中,係顯示針對實施例之添加了成核劑組成物2之樹脂組成物,在示差掃描熱量測定中所獲得之DSC曲線Q=f(θ)之對應於第2次之昇溫過程之部分之曲線圖,圖2中,係顯示針對實施例之添加了成核劑組成物2之樹脂組成物,將DSC曲線Q=f(θ)之對應於第2次之昇溫過程之部分進行基準線補正後之DSC曲線Q’=h(θ)=f(θ)-g(θ)之曲線圖。
<特性評估>
將實施例1~13及比較例1~10之樹脂組成物團塊成型所獲得之成型品之力學的特性,係依據下述內容,藉由測定彎曲彈性模數及夏比衝撃強度來進行評估。
(彎曲彈性模數)
將實施例1~13及比較例1~10之樹脂組成物團塊於80℃下乾燥8小時後,使用射出成型機(東芝機械公司製、EC-220),以樹脂溫度230℃、模具溫度40℃之條件進行射出成型,製作80mm×10mm×4mm之彎曲試驗片。將該試驗片於溫度23℃、濕度50%之恆溫恆濕槽內中靜置48小時後,由恆溫恆濕槽取出試驗片,使用彎曲試驗機(島津製作所製、AG-IS),依據ISO178測定試驗片之彎曲彈性模數(MPa)。結果併記於表5~9。
(夏比衝撃強度)
將實施例1~13及比較例1~10之樹脂組成物團塊於80℃下乾燥8小時後,藉由射出成型機(裝置;日精樹脂工業公司製、橫型射出成型機 NEX80),以樹脂溫度230℃、模具溫度40℃之加工條件成型,製作中央部具有V字型缺口之80mm×10mm×4mm之夏比衝撃強度測定用試驗片。將該試驗片靜置於溫度23℃、濕度60%之恆溫恆濕槽內7天後,由恆溫恆濕槽取出試驗片,並依據ISO179-1來測定試驗片之夏比衝撃強度(kJ/m
2)。結果併記於表5~9。
根據表5~9所示之結果,實施例1~13之樹脂組成物係具備優良的剛性及優良的耐衝撃性。另一方面,比較例1~10之樹脂組成物係不能說是具有充分的剛性或耐衝撃性者。
根據以上內容,係已確認依據本發明之成核劑組成物,可賦予包含聚烯烴系樹脂之成型品優良的力學的特性。
[圖1]係針對實施例之添加了成核劑組成物2之樹脂組成物,在示差掃描熱量測定中所獲得之DSC曲線Q=f(θ)之對應於第2次之昇溫過程之部分之曲線圖。
[圖2]係針對實施例之添加了成核劑組成物2之樹脂組成物,將DSC曲線Q=f(θ)之對應於第2次之昇溫過程之部分進行基準線補正後之DSC曲線Q’=h(θ)=f(θ)-g(θ)之曲線圖。
Claims (10)
- 一種成核劑組成物,其中包含至少一種聚烯烴系樹脂用成核劑,且 藉由以下之方法所算出之β晶分率為0.2~71%; <β晶分率之算出方法> (1)依據JIS K 7210,摻合以溫度230℃、荷重2.16kg之條件所測定出之熔體流動速率為8g/10分之均聚聚丙烯(homopolypropylene)100質量份、前述成核劑組成物0.10質量份、四[亞甲基-3-(3’,5’-tert-丁基-4’-羥基苯基)丙酸酯]甲烷0.05質量份、三(2,4-二-tert-丁基苯基)亞磷酸酯)0.1質量份及硬脂酸鈣0.05質量份,使用FM混合機混合1分鐘,獲得樹脂摻合物; (2)使用雙軸擠壓機,將前述樹脂摻合物以熔融溫度230℃進行熔融混練,並將所獲得之熔融混練物進行造粒,獲得團塊; (3)在使前述團塊以80℃乾燥8小時後,由乾燥後之團塊取樣出10mg之試料,導入示差掃描熱量測定裝置中; (4)使用前述示差掃描熱量測定裝置,將前述試料以自25℃起以50℃/min之速度昇溫至230℃為止,於230℃下保持20分鐘後,以100℃/min之速度冷卻至50℃為止,並於50℃下保持20分鐘後,以30℃/min之速度昇溫至230℃為止之溫度程序來進行示差掃描熱量測定,並將橫軸設為溫度θ(℃)、縱軸設為熱流量Q(mW),獲得DSC曲線Q=f(θ);此處,針對縱軸,係將吸熱設為正的方向; (5)於前述DSC曲線之對應於前述溫度程序中之第2次之昇溫過程之部分中,由f(θ)將基準線g(θ)=(f(200)-f(110))/90×(θ-110)+f(110)扣除,獲得經基準線補正之DSC曲線Q’=h(θ)=f(θ)-g(θ); (6)將由曲線Q’=h(θ)之110≦θ≦200之部分及連結點A(110,0)及點B(200,0)之線段AB所包圍之領域之面積設為S t;此處,S t係以下述公式表示: (7)將曲線Q’=h(θ)上之110≦θ≦200之範圍中之2個極大點設為R(θ β,h(θ β)),S(θ α,h(θ α))(惟θ β<θ α),並將曲線Q’=h(θ)上之θ β<θ<θ α之範圍中之極小點設為C(θ γ,h(θ γ);然後,通過點C,拉出與曲線Q’=h(θ)在110<θ<θ β之範圍內相接觸之切線,並將接點設為點D(θ δ,h(θ δ);然後,係將由曲線Q’=h(θ)之θ δ≦θ≦θ γ之部分及連結點D及點C之線段DC所包圍之領域之面積設為S β; 此處,S β係以下述公式表示: 惟,j(θ)=h(θ)-i(θ),i(θ)=(h(θ γ)-h(θ δ))/(θ γ-θ δ)×(θ-θ γ)+ h(θ γ); (8)由前述S t及前述S β,藉由下述公式來算出β晶分率(%): β晶分率=S β/S t×100(%)。
- 如請求項1記載之成核劑組成物,其中,包含促進聚烯烴系樹脂之α晶形成之α晶成核劑。
- 如請求項1或2記載之成核劑組成物,其中,包含促進聚烯烴系樹脂之β晶形成之β晶成核劑。
- 如請求項3記載之成核劑組成物,其中,前述β晶成核劑係包含由羧酸金屬鹽及喹吖酮化合物所成之群所選出之至少一種。
- 一種樹脂組成物,其係包含聚烯烴系樹脂,及 至少一種聚烯烴系樹脂用成核劑,且 藉由以下之方法所算出之β晶分率為0.2~71%; <β晶分率之算出方法> (1)在使前述樹脂組成物於80℃下乾燥8小時後,由乾燥後之團塊取樣出10mg之試料,導入示差掃描熱量測定裝置中; (2)使用前述示差掃描熱量測定裝置,將前述試料以自25℃起以50℃/min之速度昇溫至230℃為止,於230℃下保持20分鐘後,以100℃/min之速度冷卻至50℃為止,並於50℃下保持20分鐘後,以30℃/min之速度昇溫至230℃為止之溫度程序來進行示差掃描熱量測定,並將橫軸設為溫度θ(℃)、縱軸設為熱流量Q(mW),獲得DSC曲線Q=f(θ);此處,針對縱軸,係將吸熱設為正的方向; (3)於前述DSC曲線之對應於前述溫度程序中之第2次之昇溫過程之部分中,由f(θ)將基準線g(θ)=(f(200)-f(110))/90×(θ-110)+f(110)扣除,獲得經基準線補正之DSC曲線Q’=h(θ)=f(θ)-g(θ); (4)將由曲線Q’=h(θ)之110≦θ≦200之部分及連結點A(110,0)及點B(200,0)之線段AB所包圍之領域之面積設為S t;此處,S t係以下述公式表示: (5)將曲線Q’=h(θ)上之110≦θ≦200之範圍中之2個極大點設為R(θ β,h(θ β)),S(θ α,h(θ α))(惟θ β<θ α),並將曲線Q’=h(θ)上之θ β<θ<θ α之範圍中之極小點設為C(θ γ,h(θ γ);然後,通過點C,拉出與曲線Q’=h(θ)在110<θ<θ β之範圍內相接觸之切線,並將接點設為點D(θ δ,h(θ δ);然後,係將由曲線Q’=h(θ)之θ δ≦θ≦θ γ之部分及連結點D及點C之線段DC所包圍之領域之面積設為S β; 此處,S β係以下述公式表示: 惟,j(θ)=h(θ)-i(θ),i(θ)=(h(θ γ)-h(θ δ))/(θ γ-θ δ)×(θ-θ γ)+ h(θ γ); (6)由前述S t及前述S β,藉由下述公式來算出β晶分率(%): β晶分率=S β/S t×100(%)。
- 如請求項5記載之樹脂組成物,其中,包含促進聚烯烴系樹脂之α晶形成之α晶成核劑。
- 如請求項5或6記載之樹脂組成物,其中,包含促進聚烯烴系樹脂之β晶形成之β晶成核劑。
- 如請求項7記載之樹脂組成物,其中,前述β晶成核劑係包含由羧酸金屬鹽及喹吖酮化合物所成之群所選出之至少一種。
- 一種成型品,其係將如請求項5~8中之任一項記載之樹脂組成物成型而獲得。
- 一種樹脂組成物之製造方法,其係包含:將至少一種聚烯烴系樹脂用成核劑,以使藉由以下之方法所算出之β晶分率成為0.2~71%的方式,摻合於聚烯烴系樹脂中之摻合步驟; <β晶分率之算出方法> (1)在使前述樹脂組成物於80℃下乾燥8小時後,由乾燥後之團塊取樣出10mg之試料,導入示差掃描熱量測定裝置中; (2)使用前述示差掃描熱量測定裝置,將前述試料以自25℃起以50℃/min之速度昇溫至230℃為止,於230℃下保持20分鐘後,以100℃/min之速度冷卻至50℃為止,並於50℃下保持20分鐘後,以30℃/min之速度昇溫至230℃為止之溫度程序來進行示差掃描熱量測定,並將橫軸設為溫度θ(℃)、縱軸設為熱流量Q(mW),獲得DSC曲線Q=f(θ);此處,針對縱軸,係將吸熱設為正的方向; (3)於前述DSC曲線之對應於前述溫度程序中之第2次之昇溫過程之部分中,由f(θ)將基準線g(θ)=(f(200)-f(110))/90×(θ-110)+f(110)扣除,獲得經基準線補正之DSC曲線Q’=h(θ)=f(θ)-g(θ); (4)將由曲線Q’=h(θ)之110≦θ≦200之部分及連結點A(110,0)及點B(200,0)之線段AB所包圍之領域之面積設為S t;此處,S t係以下述公式表示: (5)將曲線Q’=h(θ)上之110≦θ≦200之範圍中之2個極大點設為R(θ β,h(θ β)),S(θ α,h(θ α))(惟θ β<θ α),並將曲線Q’=h(θ)上之θ β<θ<θ α之範圍中之極小點設為C(θ γ,h(θ γ);然後,通過點C,拉出與曲線Q’=h(θ)在110<θ<θ β之範圍內相接觸之切線,並將接點設為點D(θ δ,h(θ δ);然後,係將由曲線Q’=h(θ)之θ δ≦θ≦θ γ之部分及連結點D及點C之線段DC所包圍之領域之面積設為S β; 此處,S β係以下述公式表示: 惟,j(θ)=h(θ)-i(θ),i(θ)=(h(θ γ)-h(θ δ))/(θ γ-θ δ)×(θ-θ γ)+ h(θ γ); (6)由前述S t及前述S β,藉由下述公式來算出β晶分率(%): β晶分率=S β/S t×100(%)。
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