JP6888107B2 - ホモポリプロピレンおよびその製造方法 - Google Patents
ホモポリプロピレンおよびその製造方法 Download PDFInfo
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- JP6888107B2 JP6888107B2 JP2019546310A JP2019546310A JP6888107B2 JP 6888107 B2 JP6888107 B2 JP 6888107B2 JP 2019546310 A JP2019546310 A JP 2019546310A JP 2019546310 A JP2019546310 A JP 2019546310A JP 6888107 B2 JP6888107 B2 JP 6888107B2
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- Prior art keywords
- homopolypropylene
- residual stress
- measured
- catalyst
- produced
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- 239000000126 substance Substances 0.000 claims description 46
- 238000009826 distribution Methods 0.000 claims description 35
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- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 26
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 24
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- 125000000217 alkyl group Chemical group 0.000 claims description 21
- -1 polypropylene Polymers 0.000 claims description 21
- 239000003426 co-catalyst Substances 0.000 claims description 19
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- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 10
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 8
- DLEDOFVPSDKWEF-UHFFFAOYSA-N lithium butane Chemical compound [Li+].CCC[CH2-] DLEDOFVPSDKWEF-UHFFFAOYSA-N 0.000 description 8
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- PBKONEOXTCPAFI-UHFFFAOYSA-N 1,2,4-trichlorobenzene Chemical compound ClC1=CC=C(Cl)C(Cl)=C1 PBKONEOXTCPAFI-UHFFFAOYSA-N 0.000 description 6
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 6
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 5
- 229910052698 phosphorus Inorganic materials 0.000 description 5
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- 239000007795 chemical reaction product Substances 0.000 description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 4
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- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 3
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- KORWGADMWFSOKW-UHFFFAOYSA-N C(C)[Si](CC)=[Si](C1C(=CC2=C(C=CC=C12)C1=CC=C(C=C1)C(C)(C)C)C)C1C(=CC2=C(C=CC=C12)C1=CC=C(C=C1)C(C)(C)C)C Chemical compound C(C)[Si](CC)=[Si](C1C(=CC2=C(C=CC=C12)C1=CC=C(C=C1)C(C)(C)C)C)C1C(=CC2=C(C=CC=C12)C1=CC=C(C=C1)C(C)(C)C)C KORWGADMWFSOKW-UHFFFAOYSA-N 0.000 description 3
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- 125000000596 cyclohexenyl group Chemical group C1(=CCCCC1)* 0.000 description 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- OPRLLAPOGFQRMV-UHFFFAOYSA-N dichloromethyl-[6-[(2-methylpropan-2-yl)oxy]hexyl]silane Chemical compound C(C)(C)(C)OCCCCCC[SiH2]C(Cl)Cl OPRLLAPOGFQRMV-UHFFFAOYSA-N 0.000 description 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- UAUDZVJPLUQNMU-KTKRTIGZSA-N erucamide Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCC(N)=O UAUDZVJPLUQNMU-KTKRTIGZSA-N 0.000 description 1
- LBAQSKZHMLAFHH-UHFFFAOYSA-N ethoxyethane;hydron;chloride Chemical compound Cl.CCOCC LBAQSKZHMLAFHH-UHFFFAOYSA-N 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 125000001570 methylene group Chemical group [H]C([H])([*:1])[*:2] 0.000 description 1
- 239000003658 microfiber Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000002950 monocyclic group Chemical group 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001624 naphthyl group Chemical group 0.000 description 1
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- BKIMMITUMNQMOS-UHFFFAOYSA-N nonane Chemical compound CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 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 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 125000002255 pentenyl group Chemical group C(=CCCC)* 0.000 description 1
- 125000004344 phenylpropyl group Chemical group 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000002685 polymerization catalyst Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 125000004368 propenyl group Chemical group C(=CC)* 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000000518 rheometry Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 1
- 230000035807 sensation Effects 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 125000003107 substituted aryl group Chemical group 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 238000010557 suspension polymerization reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 description 1
- VPGLGRNSAYHXPY-UHFFFAOYSA-L zirconium(2+);dichloride Chemical compound Cl[Zr]Cl VPGLGRNSAYHXPY-UHFFFAOYSA-L 0.000 description 1
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Description
本出願は、2017年12月26日付韓国特許出願第10−2017−0180271号および2018年11月2日付韓国特許出願第10−2018−0133853号に基づいた優先権の利益を主張し、当該韓国特許出願の文献に開示されたすべての内容は本明細書の一部として含まれている。
i)分子量分布2.4未満
ii)メルトインデックス(ASTM D1238に従い230℃で2.16kg荷重で測定)5〜3000g/10min
iii)残留応力比0.5%以下
iv)190℃にて測定する角周波数(angular frequency)1rad/sでの複素粘度5〜600Pa・s、190℃にて測定する角周波数100rad/sでの複素粘度5〜300Pa・s。
X1およびX2は、それぞれ独立してハロゲンであり、
R1およびR5は、それぞれ独立してC1-20アルキルに置換されたC6-20アリールであり、
R2〜R4、およびR6〜R8は、それぞれ独立して水素、ハロゲン、C1-20アルキル、C2-20アルケニル、C1-20アルキルシリル、C1-20シリルアルキル、C1-20アルコキシシリル、C1-20エーテル、C1-20シリルエーテル、C1-20アルコキシ、C6-20アリール、C7-20アルキルアリール、またはC7-20アリールアルキルであり、
Aは、炭素、シリコンまたはゲルマニウムである。
i)分子量分布2.4未満
ii)メルトインデックス(ASTM D1238に従い230℃で2.16kg荷重で測定)5〜3000g/10min
iii)残留応力比0.5%以下
iv)190℃にて測定する角周波数1rad/sでの複素粘度5〜600Pa・s、角周波数100rad/sでの複素粘度5〜300Pa・s。
残留応力比=(RS1/RS0)*100
前記計算式1において、RS0は235℃下で前記ホモポリプロピレンに200%の変形を加えた後0.05秒未満のいずれか一つの時点(t0)における残留応力であり、RS1は235℃下でホモポリプロピレンに200%の変形を加えた後0.05秒〜1.50秒の間のいずれか一つの時点(t1)における残留応力である。
X1およびX2は、それぞれ独立してハロゲンであり、
R1およびR5は、それぞれ独立してC1-20アルキルに置換されたC6-20アリールであり、
R2〜R4、およびR6〜R8は、それぞれ独立して水素、ハロゲン、C1-20アルキル、C2-20アルケニル、C1-20アルキルシリル、C1-20シリルアルキル、C1-20アルコキシシリル、C1-20エーテル、C1-20シリルエーテル、C1-20アルコキシ、C6-20アリール、C7-20アルキルアリール、またはC7-20アリールアルキルであり、
Aは、炭素、シリコンまたはゲルマニウムである。
[化学式2]
−[Al(R11)−O]m−
前記化学式2において、
R11は互いに同一または異なってもよく、それぞれ独立してハロゲン;C1-20の炭化水素;またはハロゲンに置換されたC1-20の炭化水素であり;
mは、2以上の整数である。
(比較製造例1)
[段階1:遷移金属化合物の製造]
3L反応器にシリカ150gと10wt%のメチルアルミノキサン溶液(1214g、トルエン溶媒)を入れて95℃で24時間反応させた。沈殿後上層部は除去してトルエンで2回にかけて洗浄した。前記で製造した遷移金属化合物(9.6g)をトルエン500mlに希釈させて反応器に添加した後、50℃で5時間反応させた。反応終了後沈殿が終わると、上層部の溶液は除去して残った反応生成物をトルエンで洗浄した後ヘキサンで再び洗浄し、Atmer 163TM(CRODA社製)の帯電防止剤4.5gを入れてフィルタおよび真空乾燥して固体粒子形態のシリカ担持メタロセン触媒250gを得た。
[段階1:遷移金属化合物の製造]
前記段階1で製造した遷移金属化合物を使用することを除いては前記比較製造例1の段階2と同様の方法により行い担持触媒を製造した。
[段階1:遷移金属化合物の製造]
前記段階1で製造した遷移金属化合物を使用することを除いては前記比較製造例1の段階2と同様の方法により行い担持触媒を製造した。
[段階1:遷移金属化合物の製造]
前記段階1で製造した遷移金属化合物を使用することを除いては前記比較製造例1の段階2と同様の方法により行い担持触媒を製造した。
[段階1:遷移金属化合物の製造]
前記段階1で製造した遷移金属化合物を使用することを除いては前記比較製造例1の段階2と同様の方法により行い担持触媒を製造した。
(比較例1−1)
比較製造例1で製造したシリカ担持触媒の存在下で、連続的な2器のループ反応器を用いてプロピレンのバルク−スラリー重合を行った。
比較製造例2で製造したシリカ担持触媒の存在下で、連続的な2器のループ反応器を用いてプロピレンのバルク−スラリー重合を行った。
比較製造例2で製造したシリカ担持触媒の存在下で、連続的な2器のループ反応器を用いてプロピレンのバルク−スラリー重合を行った。
この時、トリエチルアルミニウム(TEAL)および水素気体は、それぞれポンプを用いて50ppmおよび550ppmの含有量で投入し、バルク−スラリー重合のために比較製造例2で製造したシリカ担持触媒を16.7重量%の含有量になるようにオイルおよびグリースに混ぜたマッド触媒形態で使用した。反応器の温度は70℃、時間当りの生産量は概ね38kgで運転した。プロピレン投入量は82kg/hとして重合工程によってホモポリプロピレンを製造した。
比較製造例3で製造したシリカ担持触媒の存在下で、連続的な2器のループ反応器を用いてプロピレンのバルク−スラリー重合を行った。
比較製造例3で製造したシリカ担持触媒の存在下で、連続的な2器のループ反応器を用いてプロピレンのバルク−スラリー重合を行った。
前記製造例1で製造したシリカ担持触媒の存在下で、連続的な2器のループ反応器を用いてプロピレンのバルク−スラリー重合を行った。
前記製造例1で製造したシリカ担持メタロセン触媒の存在下で、連続的な2器のループ反応器を用いてプロピレンのバルク−スラリー重合を行った。
前記実施例1−1で水素を210ppmの含有量で投入することを除いては前記実施例1−1と同様の方法により行いホモポリプロピレンを製造した。
先に、実施例1−1と、比較例1−2のホモポリプロピレン(PP)の13C NMR分析結果を図1に示した。
また、実施例1−1ないし1−3と、比較例1−1ないし1−5の各重合工程で使用された触媒の活性を評価し、その結果を下記表1に示した。
前記実施例および比較例で製造したホモポリプロピレンに対して、それぞれ試料を取って235℃下で200%の変形(strain)を加えた後10分間残留応力の変化を測定した。
[計算式1]
残留応力比(Y)=(RS1/RS0)*100
前記計算式1において、RS0は235℃下で合成樹脂試料に200%の変形を加えた後0.02秒(t0)における残留応力であり、RS1は235℃下で合成樹脂試料に200%の変形を加えた後1.00秒(t1)における残留応力である。
測定しようとするホモポリプロピレンの温度を200℃まで増加させた後、5分間その温度に維持し、その後30℃まで落とし、再び温度を増加させてDSC(Differential Scanning Calorimeter,TA社製)曲線の頂点を融点とした。この時、温度の上昇と下降の速度は10℃/minであり、融点は二番目の温度が上昇する区間で測定した結果を使用した。
(実施例2−1)
前記製造例1で製造したシリカ担持触媒の存在下で、連続的な2器のループ反応器を用いてプロピレンのバルク−スラリー重合を行った。
下記表2に記載した条件で行うことを除いては、前記実施例2−1と同様の方法により行いホモプロピレンを製造した。
Z/Nホモポリプロピレンとして市販のH7910R(LG化学社製)を使用した。
下記表2に記載した条件で行うことを除いては、前記実施例2−1と同様の方法により行いホモプロピレンを製造した。
実施例2−1ないし2−3、および比較例2−1および2−2で製造したホモポリプロピレンに対し、前記試験例2と同様の方法により物性の評価を行った。その結果を下記表3に示した。
<不織布の製造>
実施例2−1ないし2−3、および比較例2−1および2−2によるホモポリプロピレンを含む樹脂組成物を用いてメルトブロー工程を行いスパンボンド不織布を製造した。
前記実施例2−1ないし2−3、および比較例2−1および2−2によるホモポリプロピレンを用いて製造したそれぞれのスパンボンド不織布に対し、下記のような方法で物性評価を行い、その結果を下記表4に示した。
製造した不織布重量を測定して単位面積当たりの不織布重量を算出した。
不織布製造時の繊維の断糸発生の有無を確認し、下記基準に従い不織布の加工性を評価した。
<評価基準>
良好:繊維の断糸発生率が10%以下、すなわち繊維を生産する24時間を基準に、断糸発生により繊維を生産できない時間が2.4時間以下である場合
不良:繊維の断糸発生率が10%超、すなわち繊維を生産する24時間を基準に、断糸発生により繊維を生産できない時間が2.4時間超である場合
米国材料試験学会ASTM D 5035:2011(2015)方法に従い5cm幅カットストリップ法(Cut−strip)によって不織布の縦方向(MD,machine direction)と横方向(CD,cross direction)に対する強度(Strength,N/5cm)を測定した
10人のブラインドパネルの評価によって不織布の粗さを測定し、下記基準により評価した:
<評価基準>
◎◎:不織布の感触に対し粗いという評価が9人以上の場合は優れると判断
◎○:不織布の感触に対し粗いという評価が8〜7人の場合は優れると判断
◎:不織布の感触に対し粗いという評価が6〜5人の場合は優れると判断
○:不織布の感触に対し粗いという評価が4人の場合は良好であると判断
△:不織布の感触に対し粗いという評価が3ないし2人の場合は不良と判断
Х:不織布の感触に対し粗いという評価が1人以下の場合は不良と判断
Claims (19)
- 下記i)〜iv)の条件を満たし、
i)分子量分布2.21以上2.4未満
ii)メルトインデックス(ASTM D1238に従い230℃で2.16kg荷重で測定)9〜1500g/10min
iii)残留応力比0.03〜0.399%
iv)190℃にて測定する角周波数1rad/sでの複素粘度(complex viscosity)11.1〜540Pa・s、角周波数100rad/sでの複素粘度10.9〜253Pa・s、
前記残留応力比は、下記計算式1により算出する、ホモポリプロピレン。
[計算式1]
残留応力比(Y)=(RS 1 /RS 0 )*100
前記計算式1において、RS 0 は235℃下で合成樹脂試料に200%の変形を加えた後0.02秒(t 0 )における残留応力であり、RS 1 は235℃下で合成樹脂試料に200%の変形を加えた後1.00秒(t 1 )における残留応力である。 - 前記メルトインデックス(ASTM D1238に従い230℃で2.16kg荷重で測定)が9g/10min以上、200g/10min未満であり、残留応力比が0.2〜0.399%である、請求項1に記載のホモポリプロピレン。
- 前記メルトインデックス(ASTM D1238に従い230℃で2.16kg荷重で測定)が200〜1500g/10minであり、残留応力比が0.03〜0.1%である、請求項1に記載のホモポリプロピレン。
- 前記メルトインデックス(ASTM D1238に従い230℃で2.16kg荷重で測定)が9〜70g/10minであり、190℃にて測定する角周波数1rad/sでの複素粘度が430〜540Pa・sであり、190℃にて測定する角周波数100rad/sでの複素粘度180〜253Pa・sである、請求項1または2に記載のホモポリプロピレン。
- 前記メルトインデックス(ASTM D1238に従い230℃で2.16kg荷重で測定)が70g/10min超、1500g/10min以下であり、190℃にて測定する角周波数1rad/sでの複素粘度が11.1〜200Pa・sであり、190℃にて測定する角周波数100rad/sでの複素粘度10.9〜150Pa・sである、請求項1に記載のホモポリプロピレン。
- 重量平均分子量が30,000〜300,000g/molである、請求項1ないし5のいずれか一項に記載のホモポリプロピレン。
- 融点(Tm)が155〜160℃である、請求項1ないし6のいずれか一項に記載のホモポリプロピレン。
- キシレン可溶分が0.1〜1.0重量%である、請求項1ないし7のいずれか一項に記載のホモポリプロピレン。
- 前記分子量分布が2.21〜2.35である、請求項1ないし8のいずれか一項に記載のホモポリプロピレン。
- 下記i)〜iv)の条件を満たすホモポリプロピレンの製造方法であって、
i)分子量分布2.4未満、
ii)メルトインデックス(ASTM D1238に従い230℃で2.16kg荷重で測定)5〜3000g/10min、
iii)残留応力比0.5%以下、
iv)190℃にて測定する角周波数1rad/sでの複素粘度(complex viscosity)5〜600Pa・s、角周波数100rad/sでの複素粘度5〜300Pa・s、
前記残留応力比は、下記計算式1により算出しており、
[計算式1]
残留応力比(Y)=(RS 1 /RS 0 )*100
前記計算式1において、RS 0 は235℃下で合成樹脂試料に200%の変形を加えた後0.02秒(t 0 )における残留応力であり、RS 1 は235℃下で合成樹脂試料に200%の変形を加えた後1.00秒(t 1 )における残留応力であり、
シリカ担体;およびシリカ担体上に担持された下記化学式1の化合物と、助触媒を含む担持触媒の存在下で、プロピレン単量体を重合する段階を含む、ホモポリプロピレンの製造方法:
X1およびX2は、それぞれ独立してハロゲンであり、
R1およびR5は、それぞれ独立してC1-20アルキルに置換されたC6-20アリールであり、
R2〜R4、およびR6〜R8は、それぞれ独立して水素、ハロゲン、C1-20アルキル、C2-20アルケニル、C1-20アルキルシリル、C1-20シリルアルキル、C1-20アルコキシシリル、C1-20エーテル、C1-20シリルエーテル、C1-20アルコキシ、C6-20アリール、C7-20アルキルアリール、またはC7-20アリールアルキルであり、
Aは、炭素、シリコンまたはゲルマニウムである。 - 前記R1およびR5は、それぞれ独立してC3-6分枝鎖アルキル基に置換されたフェニル基である、請求項10に記載のホモポリプロピレンの製造方法。
- 前記R1およびR5は、それぞれtert−ブチルフェニルである、請求項10または11に記載のホモポリプロピレンの製造方法。
- 前記Aは、シリコンである、請求項10ないし12のいずれか一項に記載のホモポリプロピレンの製造方法。
- 前記助触媒は、下記化学式2で表される化合物を含む、請求項10ないし14のいずれか一項に記載のホモポリプロピレンの製造方法:
[化学式2]
−[Al(R11)−O]m−
前記化学式2において、
R11は互いに同一または異なってもよく、それぞれ独立してハロゲン;C1-20の炭化水素;またはハロゲンに置換されたC1-20の炭化水素であり;
mは2以上の整数である。 - 前記担持触媒は、帯電防止剤をさらに含む、請求項10ないし15のいずれか一項に記載のホモポリプロピレンの製造方法。
- 前記重合時プロピレン単量体の総重量に対し、50〜2500ppmの含有量で水素が投入される、請求項10ないし16のいずれか一項に記載のホモポリプロピレンの製造方法。
- 請求項1ないし9のいずれか一項に記載のホモポリプロピレンを含む成形品。
- 請求項1ないし9のいずれか一項に記載のホモポリプロピレンを含む不織布。
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CN110382567B (zh) | 2023-05-12 |
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