CN114716591B - 一种用于丙烯聚合的催化剂组分、制备方法及其应用 - Google Patents
一种用于丙烯聚合的催化剂组分、制备方法及其应用 Download PDFInfo
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- CN114716591B CN114716591B CN202210291479.3A CN202210291479A CN114716591B CN 114716591 B CN114716591 B CN 114716591B CN 202210291479 A CN202210291479 A CN 202210291479A CN 114716591 B CN114716591 B CN 114716591B
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- epoxycyclohexyl
- dicarboxylic acid
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- electron donor
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- 239000003054 catalyst Substances 0.000 title claims abstract description 155
- 238000006116 polymerization reaction Methods 0.000 title claims abstract description 69
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- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title abstract description 40
- 150000001875 compounds Chemical class 0.000 claims abstract description 55
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 25
- 239000001257 hydrogen Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 21
- 150000002681 magnesium compounds Chemical class 0.000 claims abstract description 17
- 150000003609 titanium compounds Chemical class 0.000 claims abstract description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 3
- -1 Lewis base compounds Chemical class 0.000 claims description 126
- UWNADWZGEHDQAB-UHFFFAOYSA-N 2,5-dimethylhexane Chemical group CC(C)CCC(C)C UWNADWZGEHDQAB-UHFFFAOYSA-N 0.000 claims description 41
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 22
- 125000004432 carbon atom Chemical group C* 0.000 claims description 22
- 125000000217 alkyl group Chemical group 0.000 claims description 19
- 125000003118 aryl group Chemical group 0.000 claims description 18
- 150000002148 esters Chemical class 0.000 claims description 15
- 125000000753 cycloalkyl group Chemical group 0.000 claims description 14
- 125000002877 alkyl aryl group Chemical group 0.000 claims description 13
- 125000003710 aryl alkyl group Chemical group 0.000 claims description 13
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 13
- 229910052736 halogen Inorganic materials 0.000 claims description 12
- 150000002367 halogens Chemical group 0.000 claims description 12
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- 125000004122 cyclic group Chemical group 0.000 claims description 4
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- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical group CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 125000001183 hydrocarbyl group Chemical group 0.000 claims 2
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- 150000003890 succinate salts Chemical class 0.000 claims 1
- 230000035945 sensitivity Effects 0.000 abstract description 3
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- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical group [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 19
- 239000000843 powder Substances 0.000 description 18
- 239000007788 liquid Substances 0.000 description 15
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 14
- 239000000203 mixture Substances 0.000 description 13
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Natural products C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
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- 238000001914 filtration Methods 0.000 description 7
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- 238000006243 chemical reaction Methods 0.000 description 6
- JQCXWCOOWVGKMT-UHFFFAOYSA-N diheptyl phthalate Chemical compound CCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCC JQCXWCOOWVGKMT-UHFFFAOYSA-N 0.000 description 6
- MQHNKCZKNAJROC-UHFFFAOYSA-N dipropyl phthalate Chemical compound CCCOC(=O)C1=CC=CC=C1C(=O)OCCC MQHNKCZKNAJROC-UHFFFAOYSA-N 0.000 description 6
- 125000004184 methoxymethyl group Chemical group [H]C([H])([H])OC([H])([H])* 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
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- 229940100539 dibutyl adipate Drugs 0.000 description 5
- 235000011147 magnesium chloride Nutrition 0.000 description 5
- 150000003254 radicals Chemical class 0.000 description 5
- ZWINORFLMHROGF-UHFFFAOYSA-N 9,9-bis(methoxymethyl)fluorene Chemical compound C1=CC=C2C(COC)(COC)C3=CC=CC=C3C2=C1 ZWINORFLMHROGF-UHFFFAOYSA-N 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 4
- KCXZNSGUUQJJTR-UHFFFAOYSA-N Di-n-hexyl phthalate Chemical compound CCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCC KCXZNSGUUQJJTR-UHFFFAOYSA-N 0.000 description 4
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Chemical compound CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 4
- 239000004593 Epoxy Substances 0.000 description 4
- SJJCABYOVIHNPZ-UHFFFAOYSA-N cyclohexyl-dimethoxy-methylsilane Chemical compound CO[Si](C)(OC)C1CCCCC1 SJJCABYOVIHNPZ-UHFFFAOYSA-N 0.000 description 4
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 4
- WGFNXLQURMLAGC-UHFFFAOYSA-N diethyl 2,3-di(propan-2-yl)butanedioate Chemical compound CCOC(=O)C(C(C)C)C(C(C)C)C(=O)OCC WGFNXLQURMLAGC-UHFFFAOYSA-N 0.000 description 4
- FLKPEMZONWLCSK-UHFFFAOYSA-N diethyl phthalate Chemical compound CCOC(=O)C1=CC=CC=C1C(=O)OCC FLKPEMZONWLCSK-UHFFFAOYSA-N 0.000 description 4
- IPKKHRVROFYTEK-UHFFFAOYSA-N dipentyl phthalate Chemical compound CCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCC IPKKHRVROFYTEK-UHFFFAOYSA-N 0.000 description 4
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- VSRWWHOJVGFSFA-UHFFFAOYSA-N (3-benzoyloxy-2-ethylpentyl) benzoate Chemical compound C=1C=CC=CC=1C(=O)OC(CC)C(CC)COC(=O)C1=CC=CC=C1 VSRWWHOJVGFSFA-UHFFFAOYSA-N 0.000 description 3
- HZXMLBSUEZTYHZ-UHFFFAOYSA-N 4-(cyclohexylmethoxy)-4-oxobutanoic acid Chemical compound OC(=O)CCC(=O)OCC1CCCCC1 HZXMLBSUEZTYHZ-UHFFFAOYSA-N 0.000 description 3
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- 238000009835 boiling Methods 0.000 description 3
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- VHPUZTHRFWIGAW-UHFFFAOYSA-N dimethoxy-di(propan-2-yl)silane Chemical compound CO[Si](OC)(C(C)C)C(C)C VHPUZTHRFWIGAW-UHFFFAOYSA-N 0.000 description 3
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- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
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- 229910052809 inorganic oxide Inorganic materials 0.000 description 1
- 125000004491 isohexyl group Chemical group C(CCC(C)C)* 0.000 description 1
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- BLQJIBCZHWBKSL-UHFFFAOYSA-L magnesium iodide Chemical compound [Mg+2].[I-].[I-] BLQJIBCZHWBKSL-UHFFFAOYSA-L 0.000 description 1
- 229910001641 magnesium iodide Inorganic materials 0.000 description 1
- BSGVJBRWDNPHOR-UHFFFAOYSA-M magnesium;butan-1-olate;chloride Chemical compound [Mg+2].[Cl-].CCCC[O-] BSGVJBRWDNPHOR-UHFFFAOYSA-M 0.000 description 1
- KRTCPMDBLDWJQY-UHFFFAOYSA-M magnesium;ethanolate;chloride Chemical compound [Mg+2].[Cl-].CC[O-] KRTCPMDBLDWJQY-UHFFFAOYSA-M 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- POPACFLNWGUDSR-UHFFFAOYSA-N methoxy(trimethyl)silane Chemical compound CO[Si](C)(C)C POPACFLNWGUDSR-UHFFFAOYSA-N 0.000 description 1
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- 150000002989 phenols Chemical class 0.000 description 1
- 239000002685 polymerization catalyst Substances 0.000 description 1
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- 150000003222 pyridines Chemical class 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
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- 239000000377 silicon dioxide Substances 0.000 description 1
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- UQMOLLPKNHFRAC-UHFFFAOYSA-N tetrabutyl silicate Chemical compound CCCCO[Si](OCCCC)(OCCCC)OCCCC UQMOLLPKNHFRAC-UHFFFAOYSA-N 0.000 description 1
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- UBZYKBZMAMTNKW-UHFFFAOYSA-J titanium tetrabromide Chemical compound Br[Ti](Br)(Br)Br UBZYKBZMAMTNKW-UHFFFAOYSA-J 0.000 description 1
- NLLZTRMHNHVXJJ-UHFFFAOYSA-J titanium tetraiodide Chemical compound I[Ti](I)(I)I NLLZTRMHNHVXJJ-UHFFFAOYSA-J 0.000 description 1
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 1
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- YEWKEJDVMCAOFM-UHFFFAOYSA-N tricyclohexylmethylsilane Chemical compound C1CCCCC1C(C1CCCCC1)([SiH3])C1CCCCC1 YEWKEJDVMCAOFM-UHFFFAOYSA-N 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical compound CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-UHFFFAOYSA-N 0.000 description 1
- FHVAUDREWWXPRW-UHFFFAOYSA-N triethoxy(pentyl)silane Chemical compound CCCCC[Si](OCC)(OCC)OCC FHVAUDREWWXPRW-UHFFFAOYSA-N 0.000 description 1
- BJDLPDPRMYAOCM-UHFFFAOYSA-N triethoxy(propan-2-yl)silane Chemical compound CCO[Si](OCC)(OCC)C(C)C BJDLPDPRMYAOCM-UHFFFAOYSA-N 0.000 description 1
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 1
- MCULRUJILOGHCJ-UHFFFAOYSA-N triisobutylaluminium Chemical compound CC(C)C[Al](CC(C)C)CC(C)C MCULRUJILOGHCJ-UHFFFAOYSA-N 0.000 description 1
- JAYPHJBLPAEMEX-UHFFFAOYSA-N trimethoxy(2-methylpentan-2-yl)silane Chemical compound CCCC(C)(C)[Si](OC)(OC)OC JAYPHJBLPAEMEX-UHFFFAOYSA-N 0.000 description 1
- HILHCDFHSDUYNX-UHFFFAOYSA-N trimethoxy(pentyl)silane Chemical compound CCCCC[Si](OC)(OC)OC HILHCDFHSDUYNX-UHFFFAOYSA-N 0.000 description 1
- LGROXJWYRXANBB-UHFFFAOYSA-N trimethoxy(propan-2-yl)silane Chemical compound CO[Si](OC)(OC)C(C)C LGROXJWYRXANBB-UHFFFAOYSA-N 0.000 description 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- 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
- C08F10/00—Homopolymers and copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F10/04—Monomers containing three or four carbon atoms
- C08F10/06—Propene
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Transition And Organic Metals Composition Catalysts For Addition Polymerization (AREA)
Abstract
本发明提供一种用于丙烯聚合的催化剂组分、制备方法及其应用,该催化剂组分包括至少一种镁化合物、至少一种钛化合物和内给电子体的原料组分,其中内给电子体采用4,5‑环氧环己基‑1,2‑二甲酸二酯类化合物或4,5‑环氧环己基‑1,2‑二甲酸二酯类化合物与另一种给电子体化合物复配,本发明由此获得的催化剂组分应用于丙烯聚合,显示出高氢调敏感性。
Description
技术领域
本发明涉及一种用于丙烯聚合的固体催化剂体系及其制备方法。具体的说,涉及一种采用4,5-环氧环己基-1,2-二甲酸二酯类化合物或其与另一种给电子体化合物复配为内给电子体来制备催化剂组分,并由此获得高氢调性能的催化剂。
背景技术
近年来对高性能聚烯烃树脂的需求越来越高,而其依赖于聚烯烃催化剂性能的不断提高。由Z-N催化剂发展可知,催化剂的发展很大程度上依赖于给电子体的发展,在催化剂制备过程中添加的内给电子体和在聚合过程中添加的外给电子体对烯烃聚合行为和聚合性能都会有很大的影响。改变催化剂中的给电子体,尤其是内给电子体,直接影响催化剂的活性中心的性质,进而影响催化剂的性能,包括活性、氢调敏感性、等规度、分子量分布等性能。为了提高催化剂的性能,近年来人们对于非邻类给电子体的研究越来越多。
目前国内外研究的非邻类的给电子体有二醚类(例如EP 0361493,EP0728724)化合物、琥珀酸酯类(例如WO9856834,WO 00063261,WO03022894)化合物以及二醇酯类(例如CN1580033,CN1580034,CN1580035)化合物等等,其中每种给电子体应用与烯烃聚合中都能改善催化剂聚合性能。
本发明研究人员在研究过程中发现,采用4,5-环氧环己基-1,2-二甲酸二酯类化合物作为内给电子体来制备用于丙烯聚合的催化剂,由此制备的催化剂在催化剂聚丙烯聚合时具有较高的氢调敏感性。
发明内容
本发明的目的在于提供了一种用于丙烯聚合的催化剂组分,其采用4,5-环氧环己基-1,2-二甲酸二酯类化合物或其与另一种给电子体复配为内给电子体,将其应用于丙烯聚合时显示出高氢调性能。
本发明的再一目的还在于提供该催化剂组分的制备方法。
本发明还一目的在于提供一种包含所述催化剂组分的丙烯聚合用催化剂。
为了实现本发明目的,本发明采用4,5-环氧环己基-1,2-二甲酸二酯类化合物或其与另一种给电子体B复配为内给电子体化合物来制备丙烯聚合用催化剂组分,并由此获得高氢调性能的丙烯聚合催化剂。
本发明提供一种用于丙烯聚合的催化剂组分,其包括如下原料组分:
1)至少一种镁化合物;
2)至少一种钛化合物;
3)4,5-环氧环己基-1,2-二甲酸二酯类化合物或4,5-环氧环己基-1,2-二甲酸二酯类化合物与另一种给电子体B化合物的复配物。
其中,所述4,5-环氧环己基-1,2-二甲酸二酯类化合物为具有通式(I)的4,5-环氧环己基-1,2-二甲酸二酯类化合物。
其中,基团R1和R2,彼此相同或不同,是C1~C20线型或支化烷基、烯基、环烷基、芳基、芳烷基或烷芳基基团,任选的包含杂原子;R3~R6彼此相同或不同,为氢或C1~C20线型或支化烷基、烯基、环烷基、芳基、芳烷基或烷芳基基团,任选的包含杂原子。
在通式(I)的给电子体中,优选R3~R6是氢或C1~C6烷基或支化烷基,R1和R2优选为C1~C15的烷基、芳基、芳烷基或烷芳基基团,更优选为C1~C8的烷基、芳基、芳烷基或烷芳基基团。
能够有利的使用的4,5-环氧环己基-1,2-二甲酸二酯类化合物的具体例子包括:
4,5环氧环己基-1,2-二甲酸二甲酯,4,5环氧环己基-1,2-二甲酸二乙酯,4,5环氧环己基-1,2-二甲酸二正丙酯,4,5环氧环己基-1,2-二甲酸二异丙酯,4,5环氧环己基-1,2-二甲酸二正丁酯,4,5环氧环己基-1,2-二甲酸二异丁酯,4,5环氧环己基-1,2-二甲酸二戊酯,4,5环氧环己基-1,2-二甲酸二异戊酯,4,5环氧环己基-1,2-二甲酸二环戊酯,4,5环氧环己基-1,2-二甲酸二己酯,4,5环氧环己基-1,2-二甲酸二庚酯,4,5环氧环己基-1,2-二甲酸二正辛酯,4,5环氧环己基-1,2-二甲酸二异辛酯,4,5环氧环己基-1,2-二甲酸二(2,2-二甲基己基)二酯,4,5环氧环己基-1,2-二甲酸二(2-二乙基己基)二酯,4,5环氧环己基-1,2-二甲酸二正壬酯,4,5环氧环己基-1,2-二甲酸二异癸酯,4,5环氧环己基-1,2-二甲酸二(2,2-二甲庚基)二酯,4,5环氧环己基-1,2-二甲酸正丁酯正戊酯,4,5环氧环己基-1,2-二甲酸正丁酯异戊酯,4,5环氧环己基-1,2-二甲酸正丁酯环戊酯,4,5环氧环己基-1,2-二甲酸正丁酯正己酯,4,5环氧环己基-1,2-二甲酸正丁酯异己基酯,4,5环氧环己基-1,2-二甲酸正丁酯(2-乙基己基)酯,4,5环氧环己基-1,2-二甲酸正戊酯正己酯,4,5环氧环己基-1,2-二甲酸正戊酯异己基酯,4,5环氧环己基-1,2-二甲酸正戊酯(2-乙基己基)酯,4,5环氧环己基-1,2-二甲酸正戊酯异壬酯,4,5环氧环己基-1,2-二甲酸正戊酯正癸酯,4,5环氧环己基-1,2-二甲酸正戊酯十一烷酯,4,5环氧环己基-1,2-二甲酸异戊酯正己酯,4,5环氧环己基-1,2-二甲酸异戊酯异己基酯,4,5环氧环己基-1,2-二甲酸异戊酯(2-乙基己基)酯,4,5环氧环己基-1,2-二甲酸异戊酯异壬酯,4,5环氧环己基-1,2-二甲酸异戊酯正癸酯,4,5环氧环己基-1,2-二甲酸正己酯(2-甲基己基)酯,4,5环氧环己基-1,2-二甲酸正己酯(2-乙基己基)酯,4,5环氧环己基-1,2-二甲酸正己酯异壬酯,4,5环氧环己基-1,2-二甲酸正己酯正癸酯,4,5环氧环己基-1,2-二甲酸正庚酯(2-乙基己基)酯,4,5环氧环己基-1,2-二甲酸正庚酯异壬酯,4,5环氧环己基-1,2-二甲酸2-乙基己基酯异壬酯,这些酯可以单独或多种混合使用;优选为:4,5环氧环己基-1,2-二甲酸二正丙酯,4,5环氧环己基-1,2-二甲酸二异丙酯,4,5环氧环己基-1,2-二甲酸二正丁酯,4,5环氧环己基-1,2-二甲酸二异丁酯,4,5环氧环己基-l,2-二甲酸二戊酯,4,5环氧环己基-1,2-二甲酸二异戊酯,4,5环氧环己基-1,2-二甲酸二环戊酯,4,5环氧环己基-1,2-二甲酸二己酯,4,5环氧环己基-1,2-二甲酸二庚酯,4,5环氧环己基-1,2-二甲酸二正辛酯,4,5环氧环己基-1,2-二甲酸二异辛酯,4,5环氧环己基-1,2-二甲酸二(2,2-二甲基己基)二酯,4,5环氧环己基-1,2-二甲酸二(2-二乙基己基)二酯。
另一种给电子体B化合物选自含有一个或多个电负性基团的Lewis碱化合物B,其中的给电子体原子选自N、O、S、P、As或Sn组成的组,优选自二醚类、酯类、二酮类和二胺类的给电子体化合物。
所述另一种给电子体B化合物与4,5-环氧环己基-1,2-二甲酸二酯类化合物复配的摩尔比为(0~100)∶1,优选为(0.01~50)∶1。
Lewis碱化合物B优选地,选自通式(II)的1,3-二醚类:
其中:R、R1、R2、R3、R4和R5可相同或不同,代表H或有1~18个碳原子的直链或支化烷基、环烷基、芳基、烷芳基或芳烷基;R6和R7可相同或不同,代表有1~20个碳原子的直链或支化烷基、3~20个碳原子的环烷基、5~20个碳原子的芳基、7~20个碳原子的烷芳基和芳烷基;R至R7中的一个或多个基团可链接形成环状结构,均可包含选自卤素、N、O、S、P和Si的一个或多个杂原子。
能够有利地使用的醚类的具体的例子包括:2-(2-乙基己基)1,3-二甲氧基丙烷,2-异丙基-1,3-二甲氧基丙烷,2-丁基-1,3-二甲氧基丙烷,2-仲丁基-1,3-二甲氧基丙烷,2-环己基-1,3-二甲氧基丙烷,2-苯基-1,3-二甲氧基丙烷,2-叔丁基-1,3-二甲氧基丙烷,2-枯基-1,3-二甲氧基丙烷,2-(2-苯基乙基)-1,3-二甲氧基丙烷,2-(2-环己基乙基)-1,3-二甲氧基丙烷,2-(对氯苯基)-1,3-二甲氧基丙烷,2-(二苯基甲基)-1,3-二甲氧基丙烷,2(1-萘基)-1,3-二甲氧基丙烷,2(对氟苯基)-1,3-二甲氧基丙烷,2(1-十氢萘基)-1,3-二甲氧基丙烷,2(对叔丁基苯基)-1,3-二甲氧基丙烷,2,2-二环己基-1,3-二甲氧基丙烷,2,2-二乙基-1,3-二甲氧基丙烷,2,2-二丙基-1,3-二甲氧基丙烷,2,2-二丁基-1,3-二甲氧基丙烷,2,2-二乙基-1,3-二乙氧基丙烷,2,2-二环戊基-1,3-二甲氧基丙烷,2,2-二丙基-1,3-二乙氧基丙烷,2,2-二丁基-1,3-二乙氧基丙烷,2-甲基-2-乙基-1,3-二甲氧基丙烷,2-甲基-2-丙基-1,3-二甲氧基丙烷,2-甲基-2-苄基-1,3-二甲氧基丙烷,2-甲基-2-苯基-1,3-二甲氧基丙烷,2-甲基-2-环己基-1,3-二甲氧基丙烷,2-甲基-2-甲基环己基-1,3-二甲氧基丙烷,2,2-双(对氯苯基)-1,3-二甲氧基丙烷,2,2-双(2-苯基乙基)-1,3-二甲氧基丙烷,2,2-双(2-环己基乙基)-1,3-二甲氧基丙烷,2-甲基-2-异丁基-1,3-二甲氧基丙烷,2-甲基-2-(2-乙基己基)-1,3-二甲氧基丙烷,2,2-双(2-乙基己基)-1,3-二甲氧基丙烷,2,2-双(对甲基苯基)-1,3-二甲氧基丙烷,2-甲基-2-异丙基-1,3-二甲氧基丙烷,2,2-二异丁基-1,3-二甲氧基丙烷,2,2-二苯基-1,3-二甲氧基丙烷,2,2-二苄基-1,3-二甲氧基丙烷,2-异丙基-2-环戊基-1,3-二甲氧基丙烷,2,2-双(环己基甲基)-1,3-二甲氧基丙烷,2,2-二异丁基-1,3-二乙氧基丙烷,2,2-二异丁基-1,3-二丁氧基丙烷,2-异丁基-2-异丙基-1,3-二甲氧基丙烷,2,2-二-仲丁基-1,3-二甲氧基丙烷,2,2-二-叔丁基-1,3-二甲氧基丙烷,2,2-二新戊基-1,3-二甲氧基丙烷,2-异-丙基-2-异戊基-1,3-二甲氧基丙烷,2-苯基-2-苄基-1,3-二甲氧_基丙烷,2-环己基-2-环己基甲基-1,3-二甲氧基丙烷。1,1-双(甲氧基甲基)-环戊二烯;1,1-双(甲氧基甲基)-2,3,4,5-四甲基环戊二烯;1,1-双(甲氧基甲基)-2,3,4,5-四苯基环戊二烯;1,1-双(甲氧基甲基)-2,3,4,5-四氟环戊二烯;1,1-双(甲氧基甲基)-3,4-二环戊基环戊二烯;1,1-双(甲氧基甲基)茚;1,1-双(甲氧基甲基)-2,3-二甲基茚;1,1-双(甲氧基甲基)-4,5,6,7-四氢茚;1,1-双(甲氧基甲基)-2,3,6,7-四氟茚;1,1-双(甲氧基甲基)-4,7-二甲基茚;1,1-双(甲氧基甲基)-3,6-二甲基茚;1,1-双(甲氧基甲基)-4-苯基茚;1,1-双(甲氧基甲基)-4-苯基-2-甲基茚;1,1-双(甲氧基甲基)-4-环己基茚;1,1-双(甲氧基甲基)-7-(3,3,3-三氟丙基)茚;1,1-双(甲氧基甲基)-7-三甲基甲硅烷基茚;1,1-双(甲氧基甲基)-7-三氟甲基茚;1,1-双(甲氧基甲基)-4,7-二甲基-4,5,6,7-四氢茚;1,1-双(甲氧基甲基)-7-甲基茚;1,1-双(甲氧基甲基)-7-环戊基茚;1,1-双(甲氧基甲基)-7-异丙基茚;1,1-双(甲氧基甲基)-7-环己基茚;1,1-双(甲氧基甲基)-7-叔丁基茚;1,1-双(甲氧基甲基)-7-叔丁基-2-甲基茚;1,1-双(甲氧基甲基)-7-苯基茚;1,1-双(甲氧基甲基)-2-苯基茚;1,1-双(甲氧基甲基)-1H-苯并[e]茚;1,1-双(甲氧基甲基)-1H-2-甲基苯并[e]茚;9,9-双(甲氧基甲基)芴;9,9-双(甲氧基甲基)-2,3,6,7-四甲基芴;9,9-双(甲氧基甲基)-2,3,4,5,6,7-六氟芴;9,9-双(甲氧基甲基)-2,3-苯并芴;9,9-双(甲氧基甲基)-2,3,6,7-二苯并芴;9,9-双(甲氧基甲基)-2,7-二异丙基芴;9,9-双(甲氧基甲基)-1,8-二氯芴;9,9-双(甲氧基甲基)-2,7-二环戊基芴;9,9-双(甲氧基甲基)-1,8-二氟芴;9,9-双(甲氧基甲基)-1,2,3,4-四氢芴;9,9-双(甲氧基甲基)-1,2,3,4,5,6,7,8-八氢芴;9,9-双(甲氧基甲基)-4-叔丁基芴。优选为:2-(2-乙基己基)1,3-二甲氧基丙烷,2-异丙基-1,3-二甲氧基丙烷,2-丁基-1,3-二甲氧基丙烷,2-苯基-1,3-二甲氧基丙烷,2-叔丁基-1,3-二甲氧基丙烷,2,2-二异丁基-1,3-二乙氧基丙烷,2,2-二异丁基-1,3-二丁氧基丙烷,2-异丁基-2-异丙基-1,3-二甲氧基丙烷,1,1-双(甲氧基甲基)茚;1,1-双(甲氧基甲基)-2,3-二甲基茚;1,1-双(甲氧基甲基)-4,5,6,7-四氢茚;9,9-双(甲氧基甲基)芴;9,9-双(甲氧基甲基)-2,3,6,7-四甲基芴,9,9-双(甲氧基甲基)-2,7-二异丙基芴;9,9-双(甲氧基甲基)-1,8-二氯芴;9,9-双(甲氧基甲基)-2,7-二环戊基芴。
Lewis碱化合物B另一优选为一元羧酸酯或多元羧酸酯类化合物,具体的例子为芳香族二元羧酸二酯化合物和脂肪族二元羧酸二酯类化合物,其中芳香族二元羧酸二酯化合物中优选邻苯二甲酸二酯或对苯二甲酸二酯。
邻苯二甲酸二酯包括:邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二正丙酯、邻苯二甲酸二异丙酯、邻苯二甲酸二正丁酯、邻苯二甲酸二异丁酯、邻苯二甲酸甲酯乙酯、邻苯二甲酸甲酯异丙酯、邻苯二甲酸甲酯正丙酯、邻苯二甲酸乙酯正丁酯、邻苯二甲酸乙酯异丁酯、邻苯二甲酸二正戊酯、邻苯二甲酸二异戊酯、邻苯二甲酸二己酯、邻苯二甲酸二正庚酯、邻苯二甲酸二正辛酯、邻苯二甲酸二异辛酯、邻苯二甲酸(2,2-二甲基己基)二酯、邻苯二甲酸(2-乙基己基)二酯、邻苯二甲酸二正壬酯、邻苯二甲酸二异癸酯、邻苯二甲酸(2,2-二甲基庚基)二酯、邻苯二甲酸正丁酯异己基酯,邻苯二甲酸正丁酯(2-乙基己基)酯、邻苯二甲酸正戊酯正己酯、邻苯二甲酸正戊酯异壬酯、邻苯二甲酸异戊酯正癸酯、邻苯二甲酸正戊酯异己基酯、邻苯二甲酸异戊基异己基酯、邻苯二甲酸正己酯(2-甲基己基酯)、邻苯二甲酸正己基(2-乙基己基酯)、邻苯二甲酸正己酯(异壬酯)、邻苯二甲酸正己基(正癸酯)、邻苯二甲酸正庚酯(2-乙基己基酯)、邻苯二甲酸正庚酯(异壬酯)、邻苯二甲酸正庚酯新壬酯和邻苯二甲酸2-乙基己酯(异壬酯)。这些酯可以单独或多种混合使用。优选为邻苯二甲酸二乙酯、邻苯二甲酸二正丙酯、邻苯二甲酸二异丙酯、邻苯二甲酸二正丁酯、邻苯二甲酸二异丁酯、邻苯二甲酸甲酯乙酯、邻苯二甲酸甲酯异丙酯、邻苯二甲酸甲酯正丙酯、邻苯二甲酸乙酯正丁酯、邻苯二甲酸乙酯异丁酯、邻苯二甲酸二正戊酯、邻苯二甲酸二异戊酯、邻苯二甲酸二己酯、邻苯二甲酸二正庚酯、邻苯二甲酸二正辛酯、邻苯二甲酸二异辛酯。
对苯二甲酸二酯包括:对苯二甲酸二甲酯、对苯二甲酸二乙酯、对苯二甲酸二正丙酯、对苯二甲酸二异丙酯、对苯二甲酸二正丁酯、对苯二甲酸二异丁酯、对苯二甲酸甲酯乙酯、对苯二甲酸甲酯异丙酯、对苯二甲酸甲酯正丙酯、对苯二甲酸乙酯正丁酯、对苯二甲酸乙酯异丁酯、对苯二甲酸二正戊酯、对苯二甲酸二异戊酯、对苯二甲酸二己酯、对苯二甲酸二正庚酯、对苯二甲酸二正辛酯、对苯二甲酸二异辛酯、对苯二甲酸(2,2-二甲基己基)二酯、对苯二甲酸(2-乙基己基)二酯、对苯二甲酸二正壬酯、对苯二甲酸二异癸酯、对苯二甲酸(2,2-二甲基庚基)二酯、对苯二甲酸正丁酯异己基酯,对苯二甲酸正丁酯(2-乙基己基)酯、对苯二甲酸正戊酯正己酯、对苯二甲酸正戊酯异壬酯、对苯二甲酸异戊酯正癸酯、对苯二甲酸正戊酯异己基酯、对苯二甲酸异戊基异己基酯、对苯二甲酸正己酯(2-甲基己基酯)、对苯二甲酸正己基(2-乙基己基酯)、对苯二甲酸正己酯(异壬酯)、对苯二甲酸正己基(正癸酯)、对苯二甲酸正庚酯(2-乙基己基酯)、对苯二甲酸正庚酯(异壬酯)、对苯二甲酸正庚酯新壬酯和对苯二甲酸2-乙基己酯(异壬酯)。这些酯可以单独或多种混合使用。优选为:对苯二甲酸二乙酯、对苯二甲酸二正丙酯、对苯二甲酸二异丙酯、对苯二甲酸二正丁酯、对苯二甲酸二异丁酯、对苯二甲酸甲酯乙酯、对苯二甲酸甲酯异丙酯、对苯二甲酸甲酯正丙酯、对苯二甲酸乙酯正丁酯、对苯二甲酸乙酯异丁酯、对苯二甲酸二正戊酯、对苯二甲酸二异戊酯、对苯二甲酸二己酯、对苯二甲酸二正庚酯、对苯二甲酸二正辛酯、对苯二甲酸二异辛酯、对苯二甲酸(2,2-二甲基己基)二酯、对苯二甲酸(2-乙基己基)二酯、对苯二甲酸二正壬酯、对苯二甲酸二异癸酯。
脂肪族二元羧酸的二酯包括:乙二酸二乙酯,乙二酸二正丙酯,乙二酸二异丙酯,乙二酸二正丁酯,乙二酸二异丁酯,乙二酸二正戊酯,乙二酸二异戊酯,乙二酸二环戊酯,乙二酸二己酯,乙二酸二正庚酯,乙二酸二正辛酯,乙二酸二异辛酯,乙二酸二(2,2-二甲基己基)酯,乙二酸二(2-乙基己基)酯,丙二酸二乙酯,丙二酸二正丙酯,丙二酸二异丙酯,丙二酸二正丁酯,丙二酸二异丁酯,丙二酸二正戊酯,丙二酸二异戊酯,丙二酸二环戊酯,丙二酸二己酯,丙二酸二正庚酯,丙二酸二正辛酯,丙二酸二异辛酯,丙二酸二(2,2-二甲基己基)酯,丙二酸二(2-乙基己基)酯,丙二酸二正壬酯,丙二酸二异癸酯,丁二酸二乙酯,丁二酸二正丙酯,丁二酸二异丙酯,丁二酸二正丁酯,丁二酸二异丁酯,丁二酸二正戊酯,丁二酸二异戊酯,丁二酸二环戊酯,丁二酸二己酯,丁二酸二正庚酯,丁二酸二正辛酯,丁二酸二异辛酯,丁二酸二(2,2-二甲基己基)酯,丁二酸二(2-乙基己基)酯,丁二酸二正壬酯,丁二酸二异癸酯,戊二酸二乙酯,戊二酸二正丙酯,戊二酸二异丙酯,戊二酸二正丁酯,戊二酸二异丁酯,戊二酸二正戊酯,戊二酸二异戊酯,戊二酸二环戊酯,戊二酸二己酯,戊二酸二正庚酯,戊二酸二正辛酯,戊二酸二异辛酯,戊二酸二(2,2-二甲基己基)酯,戊二酸二(2-乙基己基)酯,戊二酸二正壬酯,戊二酸二异癸酯,己二酸二乙酯,己二酸二正丙酯,己二酸二异丙酯,己二酸二正丁酯,己二酸二异丁酯,己二酸二正戊酯,己二酸二异戊酯,己二酸二环戊酯,己二酸二己酯,己二酸二正庚酯,己二酸二正辛酯,己二酸二异辛酯,己二酸二(2,2-二甲基己基)酯,己二酸二(2-乙基己基)酯,己二酸二正壬酯,己二酸二异癸酯,这些酯可以单独或多种混合使用。优选为:乙二酸二异丙酯,乙二酸二正丁酯,乙二酸二异丁酯,丁二酸二乙酯,丁二酸二正丙酯,丁二酸二异丙酯,丁二酸二正丁酯,丁二酸二异丁酯,己二酸二乙酯,己二酸二正丙酯,己二酸二异丙酯,己二酸二正丁酯,己二酸二异丁酯,己二酸二正戊酯,己二酸二异戊酯,己二酸二环戊酯,己二酸二己酯,己二酸二正庚酯,己二酸二正辛酯,己二酸二异辛酯。
其中多元羧酸酯类化合物中特别优选地,选自通式(III)的琥珀酸酯类化合物:
其中,基团R1和R2,彼此相同或不同,是C1~C20线型或支化烷基、链烯基、环烷基、芳基、芳烷基或烷芳基基团,任选地包含杂原子;R3~R6中至少两个基团不同于氢并且选自C1~C20线型或支化烷基、链烯基、环烷基、芳基、芳烷基或烷芳基基团,任选地含有杂原子,另外,基团R3~R6可连接在一起构成一个环。R1和R2优选是C1~C8烷基、环烷基、芳基、芳烷基和烷芳基基团。特别优选的是这样的化合物,其中R1和R2选自伯烷基,特别是支化伯烷基。合适的R1和R2的例子是甲基、乙基、正丙基、正丁基、异丁基、新戊基、2-乙基己基。特别优选的是乙基、异丁基和新戊基。
通式(III)描述的优选的化合物类别之一是这样的,其中R3~R5是氢且R6是具有3~10个碳原子的支化烷基、环烷基、芳基、芳烷基和烷芳基基团。特别优选的是这样的化合物,其中R6是具有3~10个碳原子的支化伯烷基基团或环烷基基团。合适的单取代琥珀酸酯化合物的具体例子是仲丁基琥珀酸二乙酯、己基琥珀酸二乙酯、环丙基琥珀酸二乙酯、降冰片基琥珀酸二乙酯、全氢化琥珀酸二乙酯、三甲基琥珀酸二乙酯、甲氧基琥珀酸二乙酯、对甲氧基苯基琥珀酸二乙酯、对氯苯基琥珀酸二乙酯、苯基琥珀酸二乙酯、环己基琥珀酸二乙酯、苄基琥珀酸二乙酯、环己基甲基琥珀酸二乙酯、叔丁基琥珀酸二乙酯、异丁基琥珀酸二乙酯、异丙基琥珀酸二乙酯、新戊基琥珀酸二乙酯、异戊基琥珀酸二乙酯、(1-三氟甲基乙基)琥珀酸二乙酯、芴基琥珀酸二乙酯、苯基琥珀酸(1-乙氧基羰二异丁酯)、仲丁基琥珀酸二异丁酯、己基琥珀酸二异丁酯、环丙基琥珀酸二异丁酯、降冰片基琥珀酸二异丁酯、全氢化琥珀酸二异丁酯、三甲基甲硅烷基琥珀酸二异丁酯、甲氧基琥珀酸二异丁酯、对甲氧基苯基琥珀酸二异丁酯、对氯苯氧基琥珀酸二异丁酯、环己基琥珀酸二异丁酯、苄基琥珀酸二异丁酯、环己基甲基琥珀酸二异丁酯、叔丁基琥珀酸二异丁酯、异丁基琥珀酸二异丁酯、异丙基琥珀酸二异丁酯、新戊基琥珀酸二异丁酯、异戊基琥珀酸二异丁酯、(1-三氟甲基乙基)琥珀酸二异丁酯、芴基琥珀酸二异丁酯、仲丁基琥珀酸二新戊酯、己基琥珀酸二新戊酯、环丙基琥珀酸二新戊酯、降冰片基琥珀酸二新戊酯、全氢化琥珀酸二新戊酯、三甲基甲硅烷基琥珀酸二新戊酯、甲氧基琥珀酸二新戊酯、对甲氧基苯基琥珀酸二新戊酯、对氯苯基琥珀酸二新戊酯、苯基琥珀酸二新戊酯、环己基琥珀酸二新戊酯、苄基琥珀酸二新戊酯、环己基甲基琥珀酸二新戊酯、叔丁基琥珀酸二新戊酯、异丁基琥珀酸二新戊酯、异丙基琥珀酸二新戊酯、新戊基琥珀酸二新戊酯、异戊基琥珀酸二新戊酯、(1-三氟甲基乙基)琥珀酸二新戊酯、芴基琥珀酸二新戊酯。
在通式(III)内的化合物当中另一类优选的化合物是这样的,其中R3~R6中至少两个基团不同于氢并且选自C1~C20线型或支化烷基、链烯基、环烷基、芳基、芳烷基或烷芳基基团,任选地含有杂原子。特别优选的是这样的化合物,其中两个非氢的基团连接在同一个碳原子上。合适的二取代琥珀酸酯的具体例子是:2,2-二甲基琥珀酸二乙酯、2-乙基-2-甲基琥珀酸二乙酯、2-苄基-2-异丙基琥珀酸二乙酯、2-环己基甲基-2-异丁基琥珀酸二乙酯、2-环戊基-2-正丁基琥珀酸二乙酯、2,2-二异丁基琥珀酸二乙酯、2-环己基-2-乙基琥珀酸二乙酯、2-异丙基-2-甲基琥珀酸二乙酯、2-十四烷基-2-乙基琥珀酸二乙酯、2-异丁基-2-乙基琥珀酸二乙酯、2-(1-三氟甲基乙基)-2-甲基琥珀酸二乙酯、2-异戊基-2-异丁基琥珀酸二乙酯、2-苯基-2-正丁基琥珀酸二乙酯、2,2-二甲基琥珀酸二异丁酯、2-乙基-2-甲基琥珀酸二异丁酯、2-苄基-2-异丙基琥珀酸二异丁酯、2-环己基甲基-2-异丁基琥珀酸二异丁酯、2-环戊基-2-正丁基琥珀酸二异丁酯、2,2-二异丁基琥珀酸二异丁酯、2-环己基-2-乙基琥珀酸二异丁酯、2-异丙基-2-甲基琥珀酸二异丁酯、2-十四烷基-2-乙基琥珀酸二异丁酯、2-异丁基-2-乙基琥珀酸二异丁酯、2-(1-三氟甲基乙基)-2-甲基琥珀酸二异丁酯、2-异戊基-2-异丁基琥珀酸二异丁酯、2-苯基-2-正丁基琥珀酸二异丁酯、2,2-二甲基琥珀酸二新戊酯、2-乙基-2-甲基琥珀酸二新戊酯、2-苄基-2-异丙基琥珀酸二新戊酯、2-环己基甲基-2-异丁基琥珀酸二新戊酯、2-环戊基-2-正丁基琥珀酸二新戊酯、2,2-二异丁基琥珀酸二新戊酯、2-环己基-2-乙基琥珀酸二新戊酯、2-异丙基-2-甲基琥珀酸二新戊酯、2-十四烷基-2-乙基琥珀酸二新戊酯、2-异丁基-2-乙基琥珀酸二新戊酯、2-(1-三氟甲基乙基)-2-甲基琥珀酸二新戊酯、2-异戊基-2-异丁基琥珀酸二新戊酯、2-苯基-2-正丁基琥珀酸二新戊酯。
另外,也特别优选这样的化合物,其中至少两个非氢的基团连接在不同碳原子,即R3和R5或者R4和R6。合适的化合物的具体例子是2,3-二(三甲基甲硅烷基)琥珀酸二乙酯、2-仲丁基-3-甲基琥珀酸二乙酯、2-(3,3,3-三氟丙基)-3-甲基琥珀酸二乙酯、2,3-二(2-乙基丁基)琥珀酸二乙酯、2,3-二乙基-2-异丙基琥珀酸二乙酯、2,3-二异丙基-2-甲基琥珀酸二乙酯、2,3-二环己基-2-甲基琥珀酸二乙酯、2,3-二苄基琥珀酸二乙酯、2,3-二异丙基琥珀酸二乙酯、2,3-二(环己基甲基)琥珀酸二乙酯、2,3-二叔丁基琥珀酸二乙酯、2,3-二异丁基琥珀酸二乙酯、2,3-二新戊基琥珀酸二乙酯、2,3-二异戊基琥珀酸二乙酯、2,3-二(1-三氟甲基乙基)琥珀酸二乙酯、2,3-二(十四烷基)琥珀酸二乙酯、2,3-二芴基琥珀酸二乙酯、2-异丙基-3-异丁基琥珀酸二乙酯、2-叔丁基-3-异丙基琥珀酸二乙酯、2-异丙基-3-环己基琥珀酸二乙酯、2-异戊基-3-环己基琥珀酸二乙酯、2-十四烷基-3-环己基琥珀酸二乙酯、2-环己基-3-环戊基琥珀酸二乙酯、2,2,3,3-四甲基琥珀酸二乙酯、2,2,3,3-四乙基琥珀酸二乙酯、2,2,3,3-四丙基琥珀酸二乙酯、2,3-二乙基-2,3-二异丙基琥珀酸二乙酯、2,2,3,3-四氟琥珀酸二乙酯、2,3-二(三甲基甲硅烷基)琥珀酸二异丁酯、2-仲丁基-3-甲基琥珀酸二异丁酯、2-(3,3,3-三氟丙基)-3-甲基琥珀酸二异丁酯、2,3-二(2-乙基丁基)琥珀酸二异丁酯、2,3-二乙基-2-异丙基琥珀酸二异丁酯、2,3-二异丙基-2-甲基琥珀酸二异丁酯、2,3-二环己基-2-甲基琥珀酸二异丁酯、2,3-二苄基琥珀酸二异丁酯、2,3-二异丙基琥珀酸二异丁酯、2,3-二(环己基甲基)琥珀酸二异丁酯、2,3-二叔丁基琥珀酸二异丁酯、2,3-二异丁基琥珀酸二异丁酯、2,3-二新戊基琥珀酸二异丁酯、2,3-二异戊基琥珀酸二异丁酯、2,3-二(1-三氟甲基乙基)琥珀酸二异丁酯、2,3-二(十四烷基)琥珀酸二异丁酯、2,3-二芴基琥珀酸二异丁酯、2-异丙基-3-异丁基琥珀酸二异丁酯、2-叔丁基-3-异丙基琥珀酸二异丁酯、2-异丙基-3-环己基琥珀酸二异丁酯、2-异戊基-3-环己基琥珀酸二异丁酯、2-十四烷基-3-环己基甲基琥珀酸二异丁酯、2-环己基-3-环戊基琥珀酸二异丁酯、2,2,3,3-四甲基琥珀酸二异丁酯、2,2,3,3-四乙基琥珀酸二异丁酯、2,2,3,3-四丙基琥珀酸二异丁酯、2,3-二乙基-2,3-二丙基琥珀酸二异丁酯、2,2,3,3-四氟琥珀酸二异丁酯、2,3-二(三甲基甲硅烷基)琥珀酸二新戊酯、2-仲丁基-3-甲基琥珀酸二新戊酯、2-(3,3,3-三氟丙基)-3-甲基琥珀酸二新戊酯、2,3-二(2-乙基丁基)琥珀酸二新戊酯、2,3-二乙基-2-异丙基琥珀酸二新戊酯、2,3-二异丙基-2-甲基琥珀酸二新戊酯、2,3-二环己基-2-甲基琥珀酸二新戊酯、2,3-二苄基琥珀酸二新戊酯、2,3-二异丙基琥珀酸二新戊酯、2,3-二(环己基甲基)琥珀酸二新戊酯、2,3-二叔丁基琥珀酸二新戊酯、2,3-二异丁基琥珀酸二新戊酯、2,3-二新戊基琥珀酸二新戊酯、2,3-二异戊基琥珀酸二新戊酯、2,3-(1-三氟甲基乙基)琥珀酸二新戊酯、2,3-二(十四烷基)琥珀酸二新戊酯、2,3-二芴基琥珀酸二新戊酯、2-异丙基-3-异丁基琥珀酸二新戊酯、2-叔丁基-3-异丙基琥珀酸二新戊酯、2-异丙基-3-环己基琥珀酸二新戊酯、2-异戊基-3-环己基琥珀酸二新戊酯、2-十四烷基-3-环己基甲基琥珀酸二新戊酯、2-环己基-3-环戊基琥珀酸二新戊酯、2,2,3,3-四甲基琥珀酸二新戊酯、2,2,3,3-四乙基琥珀酸二新戊酯2,2,3,3-四丙基琥珀酸二新戊酯、2,3-二乙基-2,3-二异丙基琥珀酸二新戊酯、2,2,3,3-四氟琥珀酸二新戊酯。
如同上面提到,连接在同一碳原子上的基团R3-R6中的二个或四个连接在一起构成一个环的通式(VI)的化合物也是优选的。合适的化合物的具体例子是1-(乙氧羰基)-1-(乙氧基乙酰)-2,6-二甲基环己烷、1-(乙氧羰基)-1-(乙氧基乙酰)-2,5-二甲基环戊烷、1-(乙氧羰基)-1-(乙氧基乙酰基甲基)-2-甲基环己烷、1-(乙氧羰基)-1-(乙氧基乙酰基环己基)环己烷。
上面提到的化合物可以纯异构体的形式或以对映体的混合物形式,或者以位置异构体和对映体的混合物形式使用。当要使用纯异构体时,一般采用本领域公知的常用技术将其分离出来。特别是,本发明琥珀酸酯类化合物中某些可作为纯外消旋或内消旋形式,或者替代地以这两种形式的混合物使用。
Lewis碱化合物B再一优选为选自通式(IV)的二醇酯化合物:
式中R1~R2、R3~R6为相同或不同的氢、卤素或取代或未取代的直链或支链的C1~C20烷基、C3~C20环烷基、C6~C20芳基、C7~C20烷芳基、C7~C20芳烷基、C2~C10烯烃基或C10~C20稠环芳基;但R1和R2不是氢,R3~R6及R1~R2中的一个或多个任选地成环或不成环。
所述的二醇酯类化合物具体可采用:1,3-丙二醇二苯甲酸酯、2-甲基-1,3-丙二醇二苯甲酸酯、2-乙基-1,3-丙二醇二苯甲酸酯、2-丙基-1,3-丙二醇二苯甲酸酯、2-丁基-1,3-丙二醇二苯甲酸酯、2,2-二甲基-1,3-丙二醇二苯甲酸酯、2-乙基-2-丁基-1,3-丙二醇二苯甲酸酯、2,2-二乙基-1,3-丙二醇二苯甲酸酯、2-甲基-2-丙基-1,3-丙二醇二苯甲酸酯、2-异丙基-2-异戊基-1,3-丙二醇二苯甲酸酯、2,4-戊二醇二苯甲酸酯、3-甲基-2,4-戊二醇二苯甲酸酯、3-乙基-2,4-戊二醇二苯甲酸酯、3-丙基-2,4-戊二醇二苯甲酸酯、3-丁基-2,4-戊二醇二苯甲酸酯、3,3-二甲基-2,4-戊二醇二苯甲酸酯、2-甲基-1,3-戊二醇二苯甲酸酯、2,2-二甲基-1,3-戊二醇二苯甲酸酯、2-乙基-1,3-戊二醇二苯甲酸酯、2-丁基-1,3-戊二醇二苯甲酸酯、2-甲基-1,3-戊二醇二苯甲酸酯、2-乙基-1,3-戊二醇二苯甲酸酯、2-丙基-1,3-戊二醇二苯甲酸酯、2-丁基-1,3-戊二醇二苯甲酸酯、2,2-二甲基-1,3-戊二醇二苯甲酸酯、2-甲基-1,3-戊二醇二苯甲酸酯、2,2-二甲基-1,3-戊二醇二苯甲酸酯、2-乙基-1,3-戊二醇二苯甲酸酯、2-丁基-1,3-戊二醇二苯甲酸酯、2,2,4-三甲基-1,3-戊二醇二苯甲酸酯、3-甲基-3-丁基-2,4-戊二醇二苯甲酸酯、2,2-二甲基-1,5-戊二醇二苯甲酸酯、3,5-庚二醇二苯甲酸酯、4-乙基-3,5-庚二醇二苯甲酸酯等。优选戊二醇酯和庚二醇酯。
本发明的用于烯烃聚合的催化剂组分,包含钛化合物、镁化合物和选自所述通式(I)的4,5-环氧环己基-1,2-二甲酸二酯类化合物或其与另一种给电子体B化合物的混合物。
所述的钛化合物的通式为TiXn(OR)4-n,式中R为碳原子数为1~20的烃基,X为卤素,n=0~4;所述钛化合物的通式为TiXn(OR)4-n,式中R为碳原子数为1~20的烃基,X为卤素,n=0~4;包括卤化钛、烷基卤化钛和烷氧基钛,其中卤化钛如四氯化钛、四溴化钛、四碘化钛,烷基卤化钛如甲氧基三氯化钛、乙氧基三氯化钛、丙氧基三氯化钛、正丁氧基三氯化钛、二甲氧基二氯化钛、二乙氧基二氯化钛、二丙氧基二氯化钛、二正丁氧基二氯化钛、三甲氧基氯化钛、三乙氧基氯化钛、三丙氧基氯化钛或三正丁氧基氯化钛,烷氧基钛如四乙氧基钛、四丙氧基钛、四丁氧基钛。这些钛化合物可以采用一种或多种混合使用。优选卤化钛,更优选四氯化钛。
所述镁化合物选自选自至少一种:XnMg(OR)2-n,MgCl2·mROH,R2-nMgXn,MgCl2/SiO2,MgCl2/Al2O3,或卤化镁和醇钛的混合物,式中m为0.1~6的数,0≤n≤2,X为卤素,R是氢或C1~C20的烃基;优选采用烃氧基镁化合物,二卤化镁的醇合物。具体的镁化合物可采用:氯化镁、溴化镁、碘化镁、氟化镁、甲氧基镁、乙氧基镁、丙氧基镁、丁氧基镁、异丁氧基镁、2-乙基己氧基镁、甲基甲氧基镁、甲基乙氧基镁、甲基丙氧基镁、甲基正丁氧基镁、甲基异丁氧基镁、乙基甲氧基镁、乙基乙氧基镁、乙基丙氧基镁、乙基正丁氧基镁、乙基异丁氧基镁、丙基甲氧基镁、丙基乙氧基镁、丙基丙氧基镁、丙基正丁氧基镁、丙基异丁氧基镁、正丁基甲氧基镁、正丁基乙氧基镁、正丁基丙氧基镁、正丁基正丁氧基镁、正丁基异丁氧基镁、异丁基甲氧基镁、异丁基乙氧基镁、异丁基丙氧基镁、异丁基正丁氧基镁、异丁基异丁氧基镁,氯化镁乙醇合物、氯化镁丁醇合物。
本发明的催化剂组分的制备可以按照几种方法来进行。
按照其中一种方法,用TiCl4或烃氧基钛的芳烃(例如甲苯、二甲苯等)溶液可以在-25~0℃与诸如二烷氧基镁或二芳氧基镁之类的二烃氧基镁化合物反应,并在80~130℃进行卤化。用TiCl4的芳烃溶液进行的处理可以重复一次或多次,且在多次这样的处理中一次或分批加入上述的4,5-环氧环己基-1,2-二甲酸二酯类化合物或其与另一种给电子体B复配的给电子体。
按照另一种方法,镁的醇化物或氯代醇化物和在溶液中含有上述的4,5-环氧环己基-1,2-二甲酸二酯类化合物或其与另一种给电子体B复配的给电子体的过量的TiCl4在80-135℃的温度下反应。按照优选的方法,可将通式为TiXn(OR)4-n的钛化合物,式中R为碳原子数为1~20的烃基,X为卤素,n=1~4;优选TiCl4,与从通式为MgCl2·mROH的加合物反应而制备固体催化剂组分,式中m为0.1~6的数,优选2~3.5,且R是具有1~20个碳原子的烃基。加合物可以通过以下方法适宜地制成球状:在不与加合物混溶的惰性烃存在下,将醇和氯化镁混合,使该乳液迅速急冷,从而使加合物以球形颗粒的形式固化。按照该过程制备的球形MgCl2·mROH加合物的例子描述可见于US4399054和US4469648中。如此得到的加合物可以直接与钛化合物反应,或者其可以预先经过热控制的脱醇作用(80~130℃)以得到一种加合物,其中醇的摩尔数一般低于3,优选在0.1~2.5之间。可以通过将加合物(脱醇的或其本身)悬浮在冷的TiCl4(一般-25~0℃)中来进行与钛化合物的反应;将混合物加热至80~130℃并在此温度下保持0.5~2小时。用TiCl4进行的处理可以进行一次或者多次。在用TiCl4处理期间可以加入上述的4,5-环氧环己基-1,2-二甲酸二酯类化合物或者其与第二种Lewis碱给电子体化合物B的混合物进行处理,这种处理可以重复一次或者多次。
制备本发明催化剂组分的另一种方法包括,将无水氯化镁和上述的4,5-环氧环己基-1,2-二甲酸二酯类化合物或其与另一种给电子体B复配的给电子体在二氯化镁发生活化的条件下一起研磨。如此得到的产物可以在80~130℃的温度下用过量的TiCl4处理一次或多次。处理后用烃类溶剂洗涤直至不含氯离子。按照进一步的方法,将通过对无水状态的二氯化镁、钛化合物和上述的4,5-环氧环己基-1,2-二甲酸二酯类化合物或者其与第二种Lewis碱给电子体化合物B的混合物进行共研磨而得到的产物,采用诸如1,2-二氯乙烷、氯苯、二氯甲烷之类的卤代烃进行处理。该处理在40℃至卤代烃沸点之间的温度下进行1~4个小时。然后通常用己烷之类的惰性烃类溶剂来洗涤得到产物。
按照另一种方法,将二氯化镁按照熟知的方法进行预活化,然后在约80~135℃的温度下用过量的TiCl4处理,其中在溶液中含有上述的4,5-环氧环己基-1,2-二甲酸二酯类化合物或其与另一种给电子体B复配的给电子体。用TiCl4处理多次并用己烷对固体进行清洗以除去任何未反应的TiCl4。
进一步的方法包括,还可参照CN1208045中所公开的含钛固体催化剂组分的制备方法进行制备:先在低温下在一种选自醇、酚、酮、醛、醚、胺、吡啶和酯的化合物存在下使液体镁化合物和液体钛化合物接触,沉淀出固体,接触时的温度一般为-70~200℃,优选为-30~130℃,接触过程中用上述的4,5-环氧环己基-1,2-二甲酸二酯类化合物或其与另一种给电子体B复配的给电子体处理。
本发明的催化剂组分的另一种方法包括:将镁化合物溶解于由有机环氧化合物、有机膦化合物和惰性稀释剂组成的溶剂体系中,形成均匀溶液后与钛化合物混合,在助析出剂的存在下,析出固体物;此固体物用上述的4,5-环氧环己基-1,2-二甲酸二酯类化合物或其与另一种给电子体B复配的给电子体处理,使其负载于固体物上,必要时,再用四卤化钛和惰性稀释剂处理而得到,其中助析出剂为有机酸酐、有机酸、醚、酮中的一种。所述各组分以每摩尔卤化镁计,有机环氧化合物为0.2~10摩尔,有机膦化合物为0.1~3摩尔,助析出剂为0~1.0摩尔,Ti化合物为0.5~150摩尔。
本发明的催化剂组分,还可以采用在SiO2、氧化铝等无机氧化物或多孔树脂上负载的镁化合物作为载体制备,再通过熟知的方法进行活化,然后在约80~135℃的温度下用过量的TiCl4处理,在处理过程中加入有上述的4,5-环氧环己基-1,2-二甲酸二酯类化合物或其与另一种给电子体B化合物复配的给电子体。
所述给电子体B化合物与4,5-环氧环己基-1,2-二甲酸二酯类化合物复配的摩尔比为(0~100)∶1,优选为(0.01~50)∶1。
本发明内给电子体采用4,5-环氧环己基-1,2-二甲酸二酯类化合物或其与给电子体B化合物复配时,用量为每1mol载体镁化合物中加入0.001~10mol内给电子体,优选为0.01~1mol,更优选为0.02~0.6mol。
本发明所述镁化合物与钛化合物加入量之间的摩尔比1∶0.1~100mol,优选1∶0.1~50mol。
采用本发明制备的催化剂组分可用于制备丙烯聚合用催化剂,所述的丙烯聚合用催化剂包括以下组分:
(A)本发明所述的催化剂组分(简称组分a);
(B)一种有机铝化合物(简称组分b);
(C)一种有机硅化合物(简称组分c)。
其中组分a为包含钛化合物、镁化合物和选自所述通式(I)的4,5-环氧环己基-1,2-二甲酸二酯类化合物或其与另一种给电子体B(即通式(II)、(III)、(IV)中的任意一种化合物)的混合物。
其中组分b通式为AlRmX(3-m),式中R为氢、碳原子数1~20的烃基;X为卤素,m为0≤m≤3。这些化合物包括,三乙基铝、三异丁基铝、一氯二乙基铝、二氯乙基铝、倍半乙基铝、二氯异丁基铝、一氯二异丙基铝、一氯甲基正丙基铝、一氯二苯基铝。优选三乙基铝、一氯二乙基铝、二氯乙基铝、倍半乙基铝、二氯异丁基铝以及他们任意比例的混合物。
组分c通式为SiR1 mR2 n(OR3)(4-m-n),其中,R1,R2,R3为C1~C20的烃基,R1,R2,R3可以相同可以不同,m=0~4,n=0~4。优选为,包括三甲基甲氧基硅烷、三甲基乙氧基硅烷、三正丙基甲氧基硅烷、三正丙基乙氧基硅烷、三正丁基甲氧基硅烷、三异丁基乙氧基硅烷、三环已基甲基硅烷、三环己基乙氧基硅烷、二甲基二甲氧基硅烷、二甲基二乙氧基硅烷、二正丙基二甲氧基硅烷、二异丙基二甲氧基硅烷、二正丙基二乙氧基硅烷、二异丙基二乙氧基硅烷、二正丁基二乙氧硅烷、二叔丁基二甲氧基硅烷、二正丁基二甲氧基硅烷、二异丁基二甲氧基硅烷、二叔丁基二乙氧基硅烷、正丁基甲基二甲氧基硅烷、二(2-乙基己基)二甲氧基硅烷、、二(2-乙基己基)二乙氧基硅烷、二环己基二甲氧基硅烷、二环己基二乙氧基硅烷、二环戊基二甲氧基硅烷、环己基甲基二甲氧基硅烷、环己基甲基二乙氧基硅烷、环己基乙基二甲氧基硅烷、环己基异丙基二甲氧基硅烷、环己基乙基二乙氧基硅烷、环戊基甲基二甲氧基硅烷、环戊基乙基二乙氧基硅烷、环戊基异丙基二乙氧基硅烷、环戊基异丁基二甲氧基硅烷、环己基正丙基二甲氧基硅烷、环己基正丙基二乙氧基硅烷、环己基正丁基二乙氧基硅烷、戊基甲基二甲氧基硅烷、戊基甲基二乙氧基硅烷、戊基乙基二甲氧基硅烷、戊基乙基二乙氧基硅烷、环己基二甲基甲氧基硅烷、环己基二乙基甲氧基硅烷、环己基二乙基甲氧基硅烷、环己基二乙基乙氧基硅烷、2-乙基己基二甲氧基硅烷、环己基二甲氧基硅烷、环己基二乙氧基硅烷、2-乙基己基三乙氧基硅烷、乙基三甲氧基硅烷、乙基三乙氧基硅烷、正丙基三甲氧基硅烷、正丙基三乙氧基硅烷、异丙基三甲氧基硅烷、异丙基三乙氧基硅烷、正丁基三甲氧基硅烷、异丁基三甲氧基硅烷、叔丁基三甲氧基硅烷、正丁基三乙氧基硅烷、环已基三甲氧基硅烷、环已基三乙氧基硅烷、环戊基三甲氧基硅烷、环戊基三乙氧基硅烷、乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、2-乙基己基三甲氧基硅烷、2-乙基己基三乙氧基硅烷、戊基三甲氧基硅烷、戊基三乙氧基硅烷、四甲氧基硅烷、四乙氧基硅烷、环己基环戊基二甲氧基硅烷、环己基环戊基二乙氧基硅烷、环己基环戊基二丙氧基硅烷、3-甲基环己基环戊基二甲氧基硅烷、4甲基环已基环戊基二甲氧基硅烷、3,5二甲基环已基环戊基二甲氧基硅烷、3-甲基环己基环己基二甲氧基硅烷、二(3-甲基环己基)二甲氧基硅烷、4-甲基环己基环己基二甲氧基硅烷、二(4甲基环已基)二甲氧基硅烷、3,5二甲基环已基环己基二甲氧基硅烷、二(3,5-二甲基环己基)二甲氧基硅烷、四丙氧基硅烷、四丁氧基硅烷。更为优选的,所述有机硅化合物包括环己基甲基二甲氧基硅烷、二异丙基二甲氧基硅烷、二正丁基二甲氧基硅烷、二异丁基二甲氧基硅烷、二苯基二甲氧基硅烷、苯基三乙氧基硅烷、甲基叔丁基二甲氧基硅烷、二环戊基二甲氧基硅烷、甲基苯基二甲氧基硅烷、丙基兰甲氧基硅烷、异丁基三甲氧基硅烷等。这些化合物可以单独使用或混合使用。优选为:环己基甲基二甲氧基硅烷;二异丙基二甲氧基硅烷;二正丁基二甲氧基硅烷;二异丁基二甲氧基硅烷;二苯基二甲氧基硅烷;苯基三乙氧基硅烷;甲基叔丁基二甲氧基硅烷;二环戊基二甲氧基硅烷;2-乙基哌啶基-2-叔丁基二甲氧基硅烷和(1,1,1-三氟-2-丙基)-2-乙基哌啶基二甲氧基硅烷和(1,1,1-三氟-2-丙基)-甲基而甲氧基硅烷,环己基三甲氧基硅烷;叔丁基三甲氧基硅烷和叔己基三甲氧基硅烷。
为了应用本发明中的催化剂进行丙烯聚合,均聚和共聚都可以应用上述通过组分a、b、c所制备的催化剂。组分b中的Al与组分a中的Ti的摩尔比为1~1000,优选为50~800。组分c与组分b的摩尔比为0.002~10,优选为0.01~2,最好为0.01~0.5。
各组分的加料顺序是任意的,以组分b最先加入到聚合系统中,然后加入组分c,最后加入组分a为佳。
本发明中的聚合工艺可以在有溶剂或没有溶剂的情况下进行。烯烃单体可以是气相或液相。进一步加入氢气可作为分子量调节剂。当然聚合也可以在没有分子量调节剂的情况下进行。聚合温度不要高于200℃,最好不要超过100℃。聚合压力不要超过10MPa,最好不要超过5MPa。连续聚合或分批聚合工艺都可以应用。而且聚合反应可以分一步、两步或多步进行。
本发明所述的催化剂可应用于聚丙烯的均聚或共聚。共聚的烯烃包括,直链烯烃:乙烯、1-丁烯、1-戊烯、1-己烯、1-庚烯、1-壬烯、1-癸烯;支链烯烃:3-甲基-1-丁烯和4-甲基-1-戊烯;二烯烃:丁二烯、乙烯基环戊烯和乙烯基环己烯。
本发明的催化剂组分采用4,5-环氧环己基-1,2-二甲酸二酯类化合物或其与另一种给电子体复配为内给电子体,可以实现催化剂氢调性能的提高。采用4,5-环氧环己基-1,2-二甲酸二酯类化合物或其与另一种给电子体复配为内给电子体应用于聚丙烯催化剂的制备中,改善了催化剂活性组分钛的分布,进一步对催化剂的氢调氢能加以改善。
具体实施方式
下面用实施例进一步描述本发明,有利于对本发明及其优点、效果更好的了解,但所述实施例仅用于说明本发明而不是限制本发明。
实施例中制备催化剂的操作均在高纯氮气保护下进行。具体实施例如下。
聚合物等规度的测定
采用庚烷抽提法测定(庚烷沸腾抽提6小时)。两克干燥的聚合物样品,放在抽提器中用沸腾庚烷抽提6小时后,将剩余物干燥至恒重所得的聚合物重量(g)与2的比值即为等规度。
聚合堆积密度采用GB/T 1636-2008方法测定
聚合物熔融指数采用GB/T 3682-2000方法测定
对比例1
1、固体催化剂的制备:
在500ml经氮气充分置换的带有搅拌的5口烧瓶中,加入20g二乙氧基镁载体和160ml甲苯制备悬浮液,然后维持在0℃滴加60ml甲苯与100ml四氯化钛的混合液,滴加完毕后将系统缓慢升温至80℃,加入5.4ml邻苯二甲酸二正丁酯,然后继续升温至110℃恒温1小时,然后将液体压滤干净,滤去液体,所得的固体用240ml甲苯和四氯化钛混合溶液在110℃洗涤3次。所得的固体用300ml己院在60℃洗涤4次,滤去液体并干燥,得到固体粉末即为固体催化剂,分析钛含量为2.9(wt)%,邻苯二甲酸二正丁酯含量为14.6(wt)%。
2、聚合
在5L不锈钢反应釜经氮气充分置换后,加入5ml浓度为0.5mol/L的三乙基铝己烷溶液和1mL浓度为0.1mol/L的甲基环己基二甲氧基硅烷(CMMS)己烷溶液及制备的催化剂浆液10mg,然后加入10mL己烷冲洗加料管线,再加入6L(标准状态下)氢气,和2.5L精制丙烯,控制反应在20℃预聚5分钟,升温至80℃,在此温度下聚合反应1小时。反应结束后,将反应釜降温并停搅拌排出反应产物,经干燥得到聚合物。催化剂活性为6.0万g聚丙烯/g催化剂,聚合物堆积密度为0.39g/cm3,聚合物熔融指数为19g/10min,等规度为97.5wt%。
实施例1
1、催化剂组分的制备:催化剂制备方法基本同对比例1,不同的是用7.9ml 4,5-环氧环己基-1,2二甲酸二辛酯替代邻苯二甲酸二正丁酯,得到固体粉末的催化剂。分析钛含量3.3(wt)%,4,5-环氧环己基-1,2二甲酸二辛酯为14.5(wt)%。
2、聚合:同对比例1,催化剂活性为6.3万g聚丙烯/g催化剂,聚合物堆积密度为0.38g/cm3,聚合物熔融指数为41.0g/10min,等规度为97.2wt%。
实施例2
1、催化剂组分的制备:在500ml经氮气充分置换的带有搅拌的5口烧瓶中,加入20g二乙氧基镁载体和160ml甲苯制备悬浮液,然后维持在0℃滴加60ml甲苯与100ml四氯化钛的混合液,滴加完毕后将系统缓慢升温至80℃,加入5.9ml 4,5-环氧环己基-1,2二甲酸二辛酯,然后继续升温至110℃恒温1小时,然后将液体压滤干净,滤去液体,所得的固体用240ml甲苯和四氯化钛混合溶液在110℃洗涤1次,将液体压滤干净,滤去液体。所的固体中加入240ml甲苯和四氯化钛混合溶液升温至80℃,加入2ml 4,5-环氧环己基-1,2-二甲酸二辛酯,升温至110℃恒温60min,然后将液体压滤干净,滤去液体,所得的固体用240ml甲苯和四氯化钛混合溶液在110℃洗涤再洗涤1次,然后将液体压滤干净,滤去液体,所得的固体用300ml己烷在60℃洗涤4次,滤去液体并干燥,得到固体粉末即为固体催化剂,分析钛含量为3.0(wt)%,4,5-环氧环己基-1,2-二甲酸二辛酯为15.0(wt)%。
2、聚合:同对比例1,催化剂活性为6.3万g聚丙烯/g催化剂,聚合物堆积密度为0.38g/cm3,聚合物熔融指数为34.0g/10min,等规度为97.5wt%。
实施例3
1、催化剂组分的制备:催化剂制备方法基本同对比例1,不同的是用7.9ml4,5-环氧环己基-1,2-二甲酸二正丁酯替代邻苯二甲酸二正丁酯,得到固体粉末的催化剂。分析钛含量3.4(wt)%,4,5-环氧环己基-1,2-二甲酸二正丁酯为14.0(wt)%。
2、聚合:同对比例1,催化剂活性为6.1万g聚丙烯/g催化剂,聚合物堆积密度为0.38g/cm3,聚合物熔融指数为40.0g/10min,等规度为97.2wt%。
实施例4
1、催化剂组分的制备:催化剂制备方法基本同对比例1,不同的是用7.9ml4,5-环氧环己基-1,2-二甲酸二异丁酯替代邻苯二甲酸二正丁酯,得到固体粉末的催化剂。分析钛含量3.3(wt)%,4,5-环氧环己基-1,2-二甲酸二异丁酯为14.1(wt)%。
2、聚合:同对比例1,催化剂活性为6.1万g聚丙烯/g催化剂,聚合物堆积密度为0.38g/cm3,聚合物熔融指数为40.5g/10min,等规度为97.1wt%。
实施例5
1、催化剂组分的制备:催化剂制备方法基本同对比例1,不同的是用7.9ml4,5-环氧环己基-1,2-二甲酸二乙酯替代邻苯二甲酸二正丁酯,得到固体粉末的催化剂。分析钛含量3.6(wt)%,4,5-环氧环己基-1,2-二甲酸二乙酯为13.9(wt)%。
2、聚合:同对比例1,催化剂活性为6.0万g聚丙烯/g催化剂,聚合物堆积密度为0.38g/cm3,聚合物熔融指数为40.9g/10min,等规度为97.0wt%。
实施例6
1、催化剂组分的制备:催化剂制备方法基本同对比例1,不同的是用4.3ml 4,5-环氧环己基-1,2-二甲酸二辛酯和2.2ml的邻苯二甲酸二正丁酯替代邻苯二甲酸二正丁酯,得到固体粉末的催化剂。分析钛含量3.2(wt)%,4,5-环氧环己基-1,2-二甲酸二辛酯为6.9(wt)%,邻苯二甲酸二正丁酯含量为7.1(wt)%。
2、聚合:同对比例1,催化剂活性为7.0万g聚丙烯/g催化剂,聚合物堆积密度为0.37g/cm3,聚合物熔融指数为32.2g/10min。
实施例7
1、催化剂组分的制备:催化剂制备方法基本同对比例1,不同的是用5.6ml 4,5-环氧环己基-1,2-二甲酸二辛酯和0.9ml的邻苯二甲酸二正丁酯替代邻苯二甲酸二正丁酯,得到固体粉末的催化剂。分析钛含量3.6(wt)%,4,5-环氧环己基-1,2-二甲酸二辛酯为10.8(wt)%,邻苯二甲酸二正丁酯含量为3.2(wt)%。
2、聚合:同对比例1,催化剂活性为6.9万g聚丙烯/g催化剂,聚合物堆积密度为0.37g/cm3,聚合物熔融指数为38.9g/10min。
实施例8
1、催化剂组分的制备:催化剂制备方法基本同对比例1,不同的是用4.9ml 4,5-环氧环己基-1,2-二甲酸二辛酯和1.6ml的己二酸二丁酯替代邻苯二甲酸二正丁酯,得到固体粉末的催化剂。分析钛含量3.3(wt)%,4,5-环氧环己基-1,2-二甲酸二辛酯为8.9(wt)%,己二酸二丁酯含量为6.3(wt)%。
2、聚合:同对比例1,催化剂活性为4.8万g聚丙烯/g催化剂,聚合物堆积密度为0.37g/cm3,聚合物熔融指数为26g/10min。
实施例9
1、催化剂组分的制备:催化剂制备方法基本同对比例1,不同的是用5.6ml 4,5-环氧环己基-1,2-二甲酸二辛酯和0.9ml的己二酸二丁酯替代邻苯二甲酸二正丁酯,得到固体粉末的催化剂。分析钛含量3.5(wt)%,4,5-环氧环己基-1,2-二甲酸二辛酯为10.4(wt)%,己二酸二丁酯含量为3.9(wt)%。
2、聚合:同对比例1,催化剂活性为5.3万g聚丙烯/g催化剂,聚合物堆积密度为0.37g/cm3,聚合物熔融指数为38.8g/10min。
实施例10
1、催化剂组分的制备:催化剂制备方法基本同对比例1,不同的是用4.3ml 4,5-环氧环己基-1,2-二甲酸二辛酯和2.2ml的邻苯二甲酸二异丁酯替代邻苯二甲酸二正丁酯,得到固体粉末的催化剂。分析钛含量3.5(wt)%,4,5-环氧环己基-1,2-二甲酸二辛酯为7.4(wt)%,邻苯二甲酸二异丁酯含量为6.7(wt)%。
2、聚合:同对比例1,催化剂活性为6.3万g聚丙烯/g催化剂,聚合物堆积密度为0.37g/cm3,聚合物熔融指数为33.3g/10min。
实施例11
1、催化剂组分的制备:催化剂制备方法基本同对比例1,不同的是用5.6ml 4,5-环氧环己基-1,2-二甲酸二辛酯和0.9ml的邻苯二甲酸二异丁酯替代邻苯二甲酸二正丁酯,得到固体粉末的催化剂。分析钛含量3.7(wt)%,4,5-环氧环己基-1,2-二甲酸二辛酯为10.7(wt)%,邻苯二甲酸二异丁酯含量为2.8(wt)%。
2、聚合:同对比例1,催化剂活性为6.0万g聚丙烯/g催化剂,聚合物堆积密度为0.37g/cm3,聚合物熔融指数为38.2g/10min。
实施例12
1、催化剂组分的制备:催化剂制备方法基本同对比例1,不同的是用5.6ml 4,5-环氧环己基-1,2-二甲酸二辛酯和1g的9,9-双甲氧基甲基芴替代邻苯二甲酸二正丁酯,得到固体粉末的催化剂。分析钛含量3.9(wt)%,4,5-环氧环己基-1,2-二甲酸二辛酯为10.0(wt)%,9,9-双甲氧基甲基芴含量为2.1(wt)%。
2、聚合:同对比例1,催化剂活性为6.2万g聚丙烯/g催化剂,聚合物堆积密度为0.37g/cm3,聚合物熔融指数为39.2g/10min。
实施例13
1、催化剂组分的制备:催化剂制备方法基本同对比例1,不同的是用5.6ml 4,5-环氧环己基-1,2-二甲酸二辛酯和0.9ml的2,3-二异丙基琥珀酸二乙酯替代邻苯二甲酸二正丁酯,得到固体粉末的催化剂。分析钛含量3.8(wt)%,4,5-环氧环己基-1,2-二甲酸二辛酯为10.1(wt)%,2,3-二异丙基琥珀酸二乙酯含量为2.2(wt)%。
2、聚合:同对比例1,催化剂活性为5.6万g聚丙烯/g催化剂,聚合物堆积密度为0.37g/cm3,聚合物熔融指数为37.2g/10min。
对比例2
1、催化剂组分的制备:
在500ml经氮气充分置换的带有搅拌的5口烧瓶中,在-15℃加入20gMgCl2·3C2H5OH微球和300mL四氯化钛制备悬浮液,然后维持在-15℃1小时,缓慢升温到80℃,加入3.5ml邻苯二甲酸二异丁酯,然后继续升温至110℃恒温1小时,然后将液体压滤干净,滤去液体,所得的固体用240mL四氯化钛在125℃洗涤3次。所得的固体用300mL己烷在60℃洗涤4次,滤去液体并干燥,即得到固体催化剂组分。分析钛含量3.0(wt)%,邻苯二甲酸二异丁酯为9.8(wt)%。
2、聚合:同对比例1,催化剂活性为5.2万g聚丙烯/g催化剂,聚合物堆积密度为0.45g/cm3,聚合物熔融指数为23g/10min,等规度为97.0wt%。
实施例14
1、催化剂组分的制备:同对比例2,不同的是用5ml 4,5-环氧环己基-1,2-二甲酸二辛酯代替3.5ml邻苯二甲酸二异丁酯,得到固体粉末的催化剂。分析钛含量2.9(wt)%,4,5-环氧环己基-1,2-二甲酸二辛酯为9.5(wt)%。。
2、聚合:同对比例1,催化剂活性为5.0万g聚丙烯/g催化剂,聚合物堆积密度为0.45g/cm3,聚合物熔融指数为42g/10min,等规度为96.9wt%。。
对比例3
1、催化剂组分的制备:
无水氯化镁10g、38mL癸烷和35mL的2-乙基己醇在130℃下反应2小时以形成均匀溶液。溶液中加入1.7g邻苯二甲酸酐,混合物在130℃下搅拌1小时,以使邻苯二甲酸酐完全溶解在均匀溶液中。得到的均匀溶液冷却到室温,并在1小时内滴加到保持在-20℃的200mL四氯化钛中;滴加完后混合溶液在4小时内加热到110℃,当温度达到110℃时加入3g邻苯二甲酸二正丁酯,在上述温度下搅拌2小时。反应2小时后,通过热过滤收集固体部分。固体部分悬浮在275mL四氯化钛中,在110℃条件下反应2小时。反应后,通过热过滤收集固体物部分,在110℃下用癸烷和己烷进行充分洗涤,抽干后得固体催化剂组分。
分析钛含量2.4(wt)%,邻苯二甲酸二正丁酯为9.1(wt)%。
2、聚合:同对比例1,催化剂活性为4.6万g聚丙烯/g催化剂,聚合物堆积密度为0.46g/cm3,聚合物熔融指数为22g/10min,等规度为97.3wt%。
实施例15
1、催化剂组分的制备:同对比例3,不同的是用3g 4,5-环氧环己基-1,2-二甲酸二辛酯代替邻苯二甲酸二正丁酯,得到固体粉末的催化剂。分析钛含量2.2(wt)%,4,5-环氧环己基-1,2-二甲酸二辛酯为9.0(wt)%。
2、聚合:同对比例1,催化剂活性为4.6万g聚丙烯/g催化剂,聚合物堆积密度为0.46g/cm3,聚合物熔融指数为43g/10min,等规度为97.1wt%。。
对比例4
1、催化剂组分的制备:
在500ml经氮气充分置换的带有搅拌的5口烧瓶中,室温加入10g无水氯化镁、150mL甲苯、17mL环氧氯丙烷和16mL磷酸三丁酯,搅拌下升温至50℃,并维持2小时,固体完全溶解,然后加入2.40g邻苯二甲酸酐,再维持1小时。将溶液冷却至-25℃,在1小时内滴加四氯化钛110mL,缓慢升温至80℃,在升温过程中,逐步洗出固体物。加入3g邻苯二甲酸二正丁酯,在80℃下维持1小时。过滤后200mL甲苯洗涤两次,然后加入120mL甲苯和80mL四氯化钛,继续升温到110℃,恒温2小时,然后将液体压滤干净,再重复处理一次,己烷洗涤4次,干燥后得到固体催化剂组分。
分析钛含量2.3(wt)%,邻苯二甲酸二正丁酯为9.4(wt)%。
2、聚合:同对比例1,催化剂活性为4.7万g聚丙烯/g催化剂,聚合物堆积密度为0.46g/cm3,聚合物熔融指数为21g/10min,等规度为97.5wt%。
实施例16
1、催化剂组分的制备:同对比例4,不同的是用3g 4,5-环氧环己基-1,2-二甲酸二丁酯替代邻苯二甲酸二正丁酯,得到固体粉末的催化剂。
分析钛含量2.3(wt)%,4,5-环氧环己基-1,2-二甲酸二丁酯为9.6(wt)%。
2、聚合:同对比例1,催化剂活性为4.7万g聚丙烯/g催化剂,聚合物堆积密度为0.46g/cm3,聚合物熔融指数为43g/10min,等规度为97.1wt%。
实施例17
1、催化剂组分的制备:同对比例4,不同的是用3g 4,5-环氧环己基-1,2-二甲酸二辛酯替代邻苯二甲酸二正丁酯,得到固体粉末的催化剂。分析钛含量2.3(wt)%,4,5-环氧环己基-1,2-二甲酸二辛酯为9.1(wt)%。
2、聚合:同对比例1,催化剂活性为4.7万g聚丙烯/g催化剂,聚合物堆积密度为0.46g/cm3,聚合物熔融指数为41g/10min,等规度为97.1wt%。
通过实施例数据可以看出,采用4,5-环氧环己基-1,2-二甲酸二酯类化合物单独使用或者与邻苯二甲酸二正丁酯、邻苯二甲酸二异丁酯、己二酸二丁酯、9,9-双甲氧基甲基芴、2,3-二异丙基琥珀酸二乙酯复配作为内给电子体时所得的催化剂的在相同的聚合评价条件下熔融指数明显高于以邻苯二甲酸二正丁酯等为内给电子体制得的催化剂。
通过采用4,5-环氧环己基-1,2-二甲酸二酯类化合物,或通过采用4,5-环氧环己基-1,2-二甲酸二酯类化合物与另一种给电子体化合物不同比例的复配作为内给电子体,均可以实现催化剂氢调性能的提高,此外4,5-环氧环己基-1,2-二甲酸二酯类化合物与邻苯二甲酸二正丁酯复配作为内给电子体制备的固体催化剂,在丙烯聚合时,表现出较高的活性。
本发明的范围不受所述具体实施方案的限制,所述实施方案只作为阐明本发明各个方面的单个例子,本发明范围内还包括功能等同的方法和组分。实际上,除了本文所述的内容外,本领域技术人员参照上文的描述可以容易地掌握对本发明的多种改进。所述改进也落入所附权利要求书的范围之内。
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Claims (16)
1.一种用于丙烯聚合的催化剂组分,其特征在于,其包括如下原料组分:
1)至少一种镁化合物;
2)至少一种钛化合物;
3)内给电子体:4,5-环氧环己基-1,2-二甲酸二酯类化合物或4,5-环氧环己基-1,2-二甲酸二酯类化合物与另一种给电子体B化合物的复配物;所述另一种给电子体B化合物选自含有一个或多个电负性基团的Lewis碱化合物,其中的给电子体原子选自N、O、S、P、As或Sn组成的组;
所述4,5-环氧环己基-1,2-二甲酸二酯类化合物为4,5环氧环己基-1,2-二甲酸二乙酯、4,5环氧环己基-1,2-二甲酸二正丙酯,4,5环氧环己基-1,2-二甲酸二异丙酯,4,5环氧环己基-1,2-二甲酸二正丁酯,4,5环氧环己基-1,2-二甲酸二异丁酯,4,5环氧环己基-1,2-二甲酸二戊酯,4,5环氧环己基-1,2-二甲酸二异戊酯,4,5环氧环己基-1,2-二甲酸二环戊酯,4,5环氧环己基-1,2-二甲酸二己酯,4,5环氧环己基-1,2-二甲酸二庚酯,4,5环氧环己基-1,2-二甲酸二正辛酯,4,5环氧环己基-1,2-二甲酸二异辛酯,4,5环氧环己基-1,2-二甲酸二(2,2-二甲基己基)二酯,4,5环氧环己基-1,2-二甲酸二(2-二乙基己基)二酯。
2.根据权利要求1所述的用于丙烯聚合的催化剂组分,其特征在于,所述另一种给电子体B化合物选自二醚类、酯类、二酮类和二胺类的给电子体化合物。
3.根据权利要求1或2所述的用于丙烯聚合的催化剂组分,其特征在于,所述另一种给电子体B化合物与所述4,5-环氧环己基-1,2-二甲酸二酯类化合物复配的摩尔比为(0~100):1。
4.根据权利要求3所述的用于丙烯聚合的催化剂组分,其特征在于,所述另一种给电子体B化合物与所述4,5-环氧环己基-1,2-二甲酸二酯类化合物复配的摩尔比为(0.01~50):1。
5.根据权利要求1所述的用于丙烯聚合的催化剂组分,其特征在于,每1mol载体镁化合物中加入0.001~10mol内给电子体。
6.根据权利要求5所述的用于丙烯聚合的催化剂组分,其特征在于,每1mol载体镁化合物中加入0.01~1mol内给电子体。
7.根据权利要求6所述的用于丙烯聚合的催化剂组分,其特征在于,每1mol载体镁化合物中加入0.02~0.6mol内给电子体。
8.根据权利要求1所述的用于丙烯聚合的催化剂组分,其特征在于,所述的镁化合物选自至少一种:XnMg(OR)2-n,MgCl2·mROH,R2-nMgXn,式中m为0.1-6的数,0≦n≦2,X为卤素,R是氢或C1~C20的烃基;所述钛化合物的通式为TiXn(OR)4-n,式中R为碳原子数为1~20的烃基,X为卤素,n=0~4。
9.根据权利要求2所述的用于丙烯聚合的催化剂组分,其特征在于,所述二醚类化合物选自通式(Ⅱ)的1,3-二醚类:
其中:R、R1、R2、R3、R4和R5可相同或不同,代表H或有1~18个碳原子的直链或支化烷基、环烷基、芳基、烷芳基或芳烷基;R6和R7可相同或不同,代表有1~20个碳原子的直链或支化烷基、3~20个碳原子的环烷基、5~20个碳原子的芳基、7~20个碳原子的烷芳基和芳烷基;R至R7中的一个或多个基团可链接形成环状结构,均可包含选自卤素、N、O、S、P和Si的一个或多个杂原子。
10.根据权利要求2所述的用于丙烯聚合的催化剂组分,其特征在于,所述酯类化合物为一元羧酸酯或多元羧酸酯类化合物。
11.根据权利要求10所述的用于丙烯聚合的催化剂组分,其特征在于,所述酯类化合物为芳香族二元羧酸的二酯或者脂肪族二元羧酸的二酯。
12.根据权利要求2所述的用于丙烯聚合的催化剂组分,其特征在于,所述酯类化合物选自通式(Ⅲ)的琥珀酸酯类化合物:
其中,基团R1和R2,彼此相同或不同,是C1~C20线型或支化烷基、链烯基、环烷基、芳基、芳烷基或烷芳基基团,任选地包含杂原子;R3-R6中至少两个基团不同于氢并且选自C1~C20线型或支化烷基、链烯基、环烷基、芳基、芳烷基或烷芳基基团,任选地含有杂原子,另外,基团R3~R6可连接在一起构成一个环。
13.根据权利要求2所述的用于丙烯聚合的催化剂组分,其特征在于,所述酯类化合物选自通式(Ⅳ)的二醇酯化合物:
式中R1~R2、R3~R6,彼此相同或不同,为氢、卤素或取代或未取代的直链或支链的C1~C20烷基、C3~C20环烷基、C6~C20芳基、C7~C20烷芳基、C7~C20芳烷基、C2~C10烯烃基或C10~C20稠环芳基;但当R1和R2不是氢时,R3~R6及R1~R2中的一个或多个任选地成环或不成环。
14.权利要求1-13中任一项所述的催化剂组分的制备方法,其特征在于,采用至少一种镁化合物和至少一种钛化合物与内给电子体反应制备得到,其中内给电子体采用4,5-环氧环己基-1,2-二甲酸二酯类化合物或4,5-环氧环己基-1,2-二甲酸二酯类化合物与另一种给电子体复配。
15.一种用于丙烯聚合的催化剂,其特征在于,所述的催化剂包括以下组分:
(A)权利要求1-13中任一项所述的催化剂组分,简称组分a;
(B)一种有机铝化合物,简称组分b;
(C)一种有机硅化合物,简称组分c;
其中组分b通式为AlRmX(3-m),式中R为氢、碳原子数1~20的烃基;X为卤素,m为0≤m≤3;组分c通式为SiR1 mR2 n(OR3)(4-m-n),其中,R1,R2,R3为C1~C20的烃基,R1,R2,R3可以相同可以不同,m=0~4,n=0~4。
16.权利要求1-13任一项所述的催化剂组分或权利要求15所述催化剂在丙烯聚合中的应用。
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