JP7221280B2 - シラン官能化エチレン系ポリマーの湿気硬化のためのスズ系触媒および二酸化チタンを含む組成物 - Google Patents
シラン官能化エチレン系ポリマーの湿気硬化のためのスズ系触媒および二酸化チタンを含む組成物 Download PDFInfo
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- JP7221280B2 JP7221280B2 JP2020516580A JP2020516580A JP7221280B2 JP 7221280 B2 JP7221280 B2 JP 7221280B2 JP 2020516580 A JP2020516580 A JP 2020516580A JP 2020516580 A JP2020516580 A JP 2020516580A JP 7221280 B2 JP7221280 B2 JP 7221280B2
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- silane
- ethylene
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- tin
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- 239000012190 activator Substances 0.000 description 1
- 125000004423 acyloxy group Chemical group 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 125000003282 alkyl amino group Chemical group 0.000 description 1
- XYLMUPLGERFSHI-UHFFFAOYSA-N alpha-Methylstyrene Chemical compound CC(=C)C1=CC=CC=C1 XYLMUPLGERFSHI-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 125000004104 aryloxy group Chemical group 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 125000000051 benzyloxy group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])O* 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- DQXBYHZEEUGOBF-UHFFFAOYSA-N but-3-enoic acid;ethene Chemical compound C=C.OC(=O)CC=C DQXBYHZEEUGOBF-UHFFFAOYSA-N 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 125000004369 butenyl group Chemical group C(=CCC)* 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- PBAYDYUZOSNJGU-UHFFFAOYSA-N chelidonic acid Natural products OC(=O)C1=CC(=O)C=C(C(O)=O)O1 PBAYDYUZOSNJGU-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 125000000596 cyclohexenyl group Chemical group C1(=CCCCC1)* 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 1
- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical compound CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 description 1
- 150000001993 dienes Chemical class 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000003467 diminishing effect Effects 0.000 description 1
- 229940069096 dodecene Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000001941 electron spectroscopy Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- HEAMQYHBJQWOSS-UHFFFAOYSA-N ethene;oct-1-ene Chemical compound C=C.CCCCCCC=C HEAMQYHBJQWOSS-UHFFFAOYSA-N 0.000 description 1
- BXOUVIIITJXIKB-UHFFFAOYSA-N ethene;styrene Chemical compound C=C.C=CC1=CC=CC=C1 BXOUVIIITJXIKB-UHFFFAOYSA-N 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- LDLDYFCCDKENPD-UHFFFAOYSA-N ethenylcyclohexane Chemical compound C=CC1CCCCC1 LDLDYFCCDKENPD-UHFFFAOYSA-N 0.000 description 1
- 229920001038 ethylene copolymer Polymers 0.000 description 1
- 239000012632 extractable Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 229920001002 functional polymer Polymers 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229920000578 graft copolymer Polymers 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 125000001183 hydrocarbyl group Chemical group 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000005865 ionizing radiation Effects 0.000 description 1
- 239000001282 iso-butane Substances 0.000 description 1
- 125000000555 isopropenyl group Chemical group [H]\C([H])=C(\*)C([H])([H])[H] 0.000 description 1
- 150000007517 lewis acids Chemical class 0.000 description 1
- 229920000092 linear low density polyethylene Polymers 0.000 description 1
- 239000004707 linear low-density polyethylene Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- JFNLZVQOOSMTJK-KNVOCYPGSA-N norbornene Chemical compound C1[C@@H]2CC[C@H]1C=C2 JFNLZVQOOSMTJK-KNVOCYPGSA-N 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- MSRJTTSHWYDFIU-UHFFFAOYSA-N octyltriethoxysilane Chemical compound CCCCCCCC[Si](OCC)(OCC)OCC MSRJTTSHWYDFIU-UHFFFAOYSA-N 0.000 description 1
- 229960003493 octyltriethoxysilane Drugs 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 150000001451 organic peroxides Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 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
- 239000002245 particle Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 125000000951 phenoxy group Chemical group [H]C1=C([H])C([H])=C(O*)C([H])=C1[H] 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical class OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920006124 polyolefin elastomer Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 229920005604 random copolymer Polymers 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 description 1
- SWAXTRYEYUTSAP-UHFFFAOYSA-N tert-butyl ethaneperoxoate Chemical compound CC(=O)OOC(C)(C)C SWAXTRYEYUTSAP-UHFFFAOYSA-N 0.000 description 1
- NJASUIDIZMMYED-UHFFFAOYSA-N tetra(propan-2-yl)stannane Chemical compound CC(C)[Sn](C(C)C)(C(C)C)C(C)C NJASUIDIZMMYED-UHFFFAOYSA-N 0.000 description 1
- 229920006029 tetra-polymer Polymers 0.000 description 1
- 150000003606 tin compounds Chemical class 0.000 description 1
- IUTCEZPPWBHGIX-UHFFFAOYSA-N tin(2+) Chemical compound [Sn+2] IUTCEZPPWBHGIX-UHFFFAOYSA-N 0.000 description 1
- SYRHIZPPCHMRIT-UHFFFAOYSA-N tin(4+) Chemical compound [Sn+4] SYRHIZPPCHMRIT-UHFFFAOYSA-N 0.000 description 1
- FAKFSJNVVCGEEI-UHFFFAOYSA-J tin(4+);disulfate Chemical compound [Sn+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O FAKFSJNVVCGEEI-UHFFFAOYSA-J 0.000 description 1
- 229910000375 tin(II) sulfate Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- 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
- C08F8/00—Chemical modification by after-treatment
-
- 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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K5/00—Use of organic ingredients
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/0025—Crosslinking or vulcanising agents; including accelerators
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K5/00—Use of organic ingredients
- C08K5/56—Organo-metallic compounds, i.e. organic compounds containing a metal-to-carbon bond
- C08K5/57—Organo-tin compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
- C08L23/0892—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms containing monomers with other atoms than carbon, hydrogen or oxygen atoms
-
- C—CHEMISTRY; METALLURGY
- 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
- C08F2810/00—Chemical modification of a polymer
- C08F2810/20—Chemical modification of a polymer leading to a crosslinking, either explicitly or inherently
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
Description
SIOPLAS(商標)プロセス(ケーブル押出プロセスで使用する前に別の工程で作製)、または
MONOSIL(商標)プロセス(ケーブル製造プロセス中にその場で作製-過酸化物、シランおよび触媒を含むエチレン系ポリマー組成物の、1工程の溶融混合、反応、押出による)。
米国特許実務の目的のため、参照された特許、特許出願、または刊行物の内容は、特に(この開示で具体的に提供される定義と矛盾しない範囲の)定義および当該技術分野の一般知識の開示に関して、その全体が参照により組み込まれている(またはその同等の米国版は参照により組み込まれている)。
本発明の実施において使用されるエチレン系ポリマーは、分岐、線状、または実質的に線状であり得、反応器内での重合または共重合(低圧または高圧)によって、または反応器後改質(グラフトコポリマーを作製するための反応押出成形など)により作製され得る。本明細書で使用される場合、「高圧反応器」または「高圧プロセス」という用語は、少なくとも5000ポンド/平方インチ(psi)(34.47メガパスカルまたはmPa)の圧力で動作する任意の反応器またはプロセスである。当業者に知られているように、「分岐」エチレン系ポリマーは、高圧反応器またはプロセスで調製されることが多く(しかしそれのみではないが)、ポリマー骨格と分岐自体の両方に分岐が見られる高度に分岐したポリマー構造を持つ傾向がある。対照的に、「実質的に線状」とは、1,000個の炭素原子当たり0.01~3個の長鎖分岐で置換された骨格を有するポリマーを意味する。いくつかの実施形態では、エチレン系ポリマーは、1,000個の炭素原子当たり0.01~1個の長鎖分岐、または1,000個の炭素原子当たり0.05~1個の長鎖分岐で置換される骨格を有することができる。
エチレンと効果的に共重合する、またはエチレンポリマーにグラフトして架橋する、任意のシランを本発明の実施に使用することができ、これらは、この式のみに限定されないが特定の例として以下の式によって説明される:
本発明の実施に使用される触媒組成物は、スズ系触媒と酸化チタン(IV)を含む。スズ系触媒はルイス酸であり、スズ(I)、スズ(II)、スズ(III)およびスズ(IV)のさまざまな有機誘導体が含まれるが、これらに限定されない。有機スズ化合物またはスタンナンとしても知られるこれらの化合物の例は、有機スズのハロゲン化物、水素化物、酸化物および水酸化物、高度に調整されたスタンナン、および三有機スズカチオンである。特定の触媒には、ジブチルスズジラウレート(DBTDL)、ジメチルヒドロキシスズオレエート、ジオクチルスズマレエート、ジ-n-ブチルスズマレエート、ジブチルスズジアセテート、ジブチルスズジオクトエート、酢酸第一スズおよびオクタン酸第一スズ、およびUS2008/0277137に開示されているようなジスタノキサンが含まれるが、これらに限定されない。多くが市販されており、DBTDLは好ましいスズ系触媒である。
本発明の触媒組成物およびポリマー組成物の両方は、添加剤、充填剤などを含むことができ、これらには、酸化防止剤(例えば、IRGANOX(商標)1010(ヒンダードフェノール)およびIRGAFOS(商標)168(亜リン酸塩)、両方ともCiba Specialty Chemicalsから入手可能)、UV安定剤、粘着剤(cling additive)、光安定剤(例えば、ヒンダードアミン)、可塑剤(例えば、フタル酸ジオクチルまたはエポキシ化大豆油)、熱安定剤、離型剤、粘着付与剤(例えば、炭化水素粘着付与剤)、ワックス(例えば、ポリエチレンワックス)、加工助剤(例えば、油、ステアリン酸などの有機酸、有機酸の金属塩)、着色剤および顔料、および充填剤(例えば、カーボンブラック、タルク)が含まれるが、これらに限定されない。これらの添加剤などは、処理中または最終製品として触媒組成物またはポリマー組成物の所望の物理的または機械的特性を妨げない範囲で、既知の量および既知の方法で使用される。
シラン官能化エチレンポリマー、触媒組成物および添加剤などの配合は、もしあれば、当業者に知られている標準的な手段によって実施することができる。配合機器の例は、BANBURY(商標)またはBOLLING(商標)インターナルミキサーなどのインターナルバッチミキサーである。代替的に、FARREL(商標)連続ミキサー、WERNER AND PFLEIDERER(商標)二軸スクリューミキサー、またはBUSS(商標)混練連続押出機などの連続一軸または二軸スクリューミキサーを使用することができる。使用するミキサーのタイプ、およびミキサーの動作条件は、粘度、体積抵抗率、押し出し表面の滑らかさなどのポリマー組成物の特性に影響を及ぼす。
一実施形態において、本発明のポリマー組成物は、既知の量で、既知の方法により(例えば、USP5,246,783および4,144,202に記載の機器および方法により)シースまたは絶縁層としてケーブルに適用できる。典型的には、ポリマー組成物は、ケーブル被覆ダイを備えた反応器押出機で調製され、ポリマー組成物の成分が配合された後、ケーブルがダイを通して引き出されるときにポリマー組成物がケーブル上に押し出される。硬化は反応器-押出機中で開始することができる。
高温クリープ
高温クリープ伸びは、UL2556セクション7.9に従って行われる。ダイプレスでドッグボーン形にカットすることにより、プレスしたプラック試料から3つの試料を調製する。総重量は、次式を使用して決定される。
重量=CA×29.0lbf/インチ2
式中、CA=試験片の断面積である。
C=高温クリープ伸び、%
De=得られたベンチマーク間の距離、および
G=ベンチマーク間の元の距離。
引張強度と破断点伸びは、試験片が破断する実際の最大荷重を示すデバイスを使用して、UL2556セクション3.5に従って行われる。このデバイスは、12~305mm/分の速度と設定速度の20%の精度で電動式顎(power-actuated Jaw)を操作する。ダイプレスを使用してドッグボーン形にカットすることにより、完成したプラックから3つの試料を調製する。真っ直ぐな試験片は、250±2mm(10±0.08インチ)離れた2点でゲージマークされる。試験片は、顎の間にゲージマークが付いた状態で機械の顎にグリップされ、顎は10インチ/分の速度で離れる。有効な破断がゲージマーク間で発生し、いずれかのゲージマークから25mm(1インチ)以内である。破断前の最大荷重が記録される。破断時のゲージマーク間の距離は、最も近い2mm(0.08インチ)まで記録される。
CHEMOURS(商標)R105二酸化チタン(TiO2)は、少なくとも92重量%のTiO2、3.2重量%以下のアルミナ、3.5重量%以下のシリカ、および0.2重量%以下の炭素を含む微細な乾燥粉末である。
表1および2に報告されている組成物は、カムローターを備えた420ミリリットル(mL)BRABENDER(商標)ミキシングボウルを使用して調製される。バッチ質量は、本発明に記載の各配合物でミキシングボウルの70%の充填を提供するように計算される。ミキシングボウルは150℃の設定温度に予熱され、ローター速度は毎分25回転(rpm)に設定される。ポリマーの半分をボウルに加え、ポリマーの溶融物が形成されるまで流動(flux)させる。次に、酸化チタン(IV)とカーボンブラックを含むすべての充填剤をゆっくりと添加し、ポリマー溶融物に組み込む。次に、ポリマーの残りの量と酸化防止剤を追加し、ローター速度を40rpmに上げる。バッチをさらに5分間流動させる。ミキシングボウルから取り出したら、配合物をコールドプレスに5分間入れる。得られたプラックを小さな断片にカットする。チップを、24:1押出機を備えたBRABENDER(商標)モデルPrep Mixer/Measuring Head実験室電気バッチミキサーに供給する。24:1 Maddox混練頭部付きスクリューを使用して、ストランドダイを通してポリマーを搬送および溶融する(40rpmスクリュー速度で、20/40/60/20メッシュスクリーンパックおよびゾーン1、ゾーン2、ゾーン3、およびダイにわたって150℃のフラット設定温度プロファイルを使用)。ストランド化した押出物は再度Wileyミルで粉砕されてペレットを生成する。
表8(下記)に報告されている組成物を、撹拌棒付きの25mL(5ドラム)透明ホウケイ酸ガラスバイアル中で調製する。ブチル化ヒドロキシトルエン(BHT)をバイアルに入れて目標濃度に到達させ、10mLのドデカンを加える。次に、セプタム(septum)を使用してバイアルを閉じ、窒素を使用してバイアル内の酸素を置換する。残りの手順の間、バイアルは窒素ブランケット下のままである。ドデカン中のBHTを含むバイアルを、ホットプレート上の加熱要素に置く。ホットプレートの温度は110℃に設定され、撹拌速度は500rpmに設定されている。110℃の目標温度に達したら、目標量のDBSA、ジブチルスズジラウレート、TiO2および/またはテトライソプロピルチタネートを反応混合物に加える。約100mgのアリコートを2時間かけて反応混合物から取り出し、アセトニトリルで希釈して約100の希釈比に到達させた。超高速液体クロマトグラフィー(UHPLC)を使用する定量化のために、すべての正確な重量を+/-0.0001gで記録した。
Claims (9)
- シラン官能化エチレン系ポリマーの硬化を促進するための触媒組成物であって、前記触媒組成物が、
(1)スズ系触媒と、
(2)
(i)二酸化チタン(TiO2)および
(ii)テトライソプロピルチタネートからなる群から選択される、酸化チタン(IV)と、を含み、
ただし、前記酸化チタン(IV)がテトライソプロピルチタネートである場合、触媒組成物は、前記触媒組成物の総重量に基づいて、0.5:1~1.0:0.5のスズ系触媒対テトライソプロピルチタネートの重量パーセント比を有し、かつ、前記酸化チタン(IV)が二酸化チタン(TiO 2 )である場合、スズ系触媒対TiO 2 のモル比は0.0004:0.06~0.0006:0.025である、触媒組成物。 - 前記スズ系触媒が、ジブチルスズジラウレート(DBTDL)、ジメチルヒドロキシスズオレエート、ジオクチルスズマレエート、ジ-n-ブチルスズマレエート、ジブチルスズジアセテート、ジブチルスズジオクトエート、酢酸第一スズおよびオクタン酸第一スズのうちの少なくとも1つである、請求項1に記載の触媒組成物。
- 前記酸化チタン(IV)が、二酸化チタン(TiO2)である、請求項2に記載の触媒組成物。
- 前記酸化チタン(IV)が、テトライソプロピルチタネートである、請求項2に記載の触媒組成物。
- (A)請求項1に記載の触媒組成物と、(B)担体樹脂と、を含むマスターバッチ。
- 前記担体樹脂が、シラン官能化エチレン系ポリマーのシランによるその官能化前のエチレン系ポリマーである、請求項5に記載のマスターバッチ。
- シラン官能化エチレン系ポリマーの硬化プロセスであって、(1)前記シラン官能化エチレン系ポリマーと請求項1に記載の触媒組成物を混合することによりポリマー組成物を形成する工程と、(2)前記ポリマー組成物を硬化条件にかける工程と、を含む、プロセス。
- 前記触媒組成物が、マスターバッチの形態である、請求項7に記載のプロセス。
- 前記シラン官能化エチレン系ポリマーのシラン官能性が、ビニルトリアルコキシシランの誘導体である、請求項7に記載の方法。
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