CN117567814A - 一种空心玻璃微珠母粒的制备方法 - Google Patents
一种空心玻璃微珠母粒的制备方法 Download PDFInfo
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- CN117567814A CN117567814A CN202410050015.2A CN202410050015A CN117567814A CN 117567814 A CN117567814 A CN 117567814A CN 202410050015 A CN202410050015 A CN 202410050015A CN 117567814 A CN117567814 A CN 117567814A
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- hollow glass
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- 239000011521 glass Substances 0.000 title claims abstract description 81
- 239000004005 microsphere Substances 0.000 title claims abstract description 23
- 239000004594 Masterbatch (MB) Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000011324 bead Substances 0.000 claims abstract description 63
- 239000004743 Polypropylene Substances 0.000 claims abstract description 35
- -1 polypropylene Polymers 0.000 claims abstract description 33
- 229920001155 polypropylene Polymers 0.000 claims abstract description 33
- 239000003607 modifier Substances 0.000 claims abstract description 31
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 8
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 48
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 27
- 238000002156 mixing Methods 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 22
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 22
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims description 20
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000002390 rotary evaporation Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 17
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 claims description 16
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 15
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 14
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 14
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 14
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 14
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- 238000004440 column chromatography Methods 0.000 claims description 12
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 claims description 12
- 238000010992 reflux Methods 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- 238000000967 suction filtration Methods 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000011347 resin Substances 0.000 claims description 9
- 229920005989 resin Polymers 0.000 claims description 9
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
- BITPLIXHRASDQB-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane Chemical compound C=C[Si](C)(C)O[Si](C)(C)C=C BITPLIXHRASDQB-UHFFFAOYSA-N 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 8
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- JGFBRKRYDCGYKD-UHFFFAOYSA-N dibutyl(oxo)tin Chemical compound CCCC[Sn](=O)CCCC JGFBRKRYDCGYKD-UHFFFAOYSA-N 0.000 claims description 7
- 238000004821 distillation Methods 0.000 claims description 7
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 7
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- 239000006087 Silane Coupling Agent Substances 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 6
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
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- ILWRPSCZWQJDMK-UHFFFAOYSA-N triethylazanium;chloride Chemical compound Cl.CCN(CC)CC ILWRPSCZWQJDMK-UHFFFAOYSA-N 0.000 claims description 3
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- 239000003063 flame retardant Substances 0.000 abstract description 13
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 12
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- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 4
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910010272 inorganic material Inorganic materials 0.000 description 3
- 239000011147 inorganic material Substances 0.000 description 3
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- 150000003254 radicals Chemical class 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 2
- 239000008116 calcium stearate Substances 0.000 description 2
- 235000013539 calcium stearate Nutrition 0.000 description 2
- 125000001309 chloro group Chemical group Cl* 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- 235000019359 magnesium stearate Nutrition 0.000 description 2
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 description 2
- 238000010525 oxidative degradation reaction Methods 0.000 description 2
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- 230000035939 shock Effects 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical class ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
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- 239000006227 byproduct Substances 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
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- 239000000919 ceramic Substances 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 238000012650 click reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
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- 239000006260 foam Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
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- 230000003287 optical effect Effects 0.000 description 1
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- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000003711 photoprotective effect Effects 0.000 description 1
- 239000005373 porous glass Substances 0.000 description 1
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- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
- C07F9/553—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having one nitrogen atom as the only ring hetero atom
- C07F9/576—Six-membered rings
- C07F9/59—Hydrogenated pyridine rings
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- 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
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
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Abstract
本发明公开了一种空心玻璃微珠母粒的制备方法,属于聚丙烯复合材料技术领域。通过将改性剂接枝在空心玻璃微珠表面,并通过聚合反应连接在聚丙烯分子链上,不仅改善了空心玻璃微珠与聚丙烯的相容性,而且与直接添加改性剂相比,这种方法使改性剂不易迁移和渗出,保证了性能的长久性。改性剂含有P‑N阻燃成分、‑Si‑O‑Si‑链段、受阻胺和长碳链结构,能显著提升聚丙烯的阻燃性能和一定程度的抗冲性能,还能与抗氧剂起协同作用,加强了聚丙烯的耐候耐老化性能。经空心玻璃微珠改性后的聚丙烯力学性能并未下降,并且密度较低,符合轻质化汽车领域的应用需求。
Description
技术领域
本发明属于聚丙烯母粒技术领域,具体地,涉及一种空心玻璃微珠母粒的制备方法。
背景技术
玻璃微珠是直径在数微米至数毫米粒径范围内的玻璃(或陶瓷)球体,具有光学性能好、球形透镜特性、抗冲击性能强、滚动性好、导热系数低、质轻等特点,已广泛用于城市交通标志、汽车牌号、回射幕布、喷吹技术、填充材料、保温材料等领域。
常见的玻璃微珠有实心、空心、多孔玻璃微珠之分,其中空心玻璃微珠,是一种中空的,内含惰性气体的微小圆球状粉末,具有重量轻、体积大、导热系数低、抗压强度高、分散性、流动性、稳定性好的优点。因其出色的性能,经常被作为塑料的填充材料,大幅降低塑料制品的密度,同时提高材料模量,减小材料翘曲。另外,空心玻璃微珠为一种填料的独到之处在于它为球形且表面光滑,它们像轴承一样互相之间能够滚动,具有很好的自由流动性。
聚丙烯(简称为PP),具有成本低、轻质、易加工、可回收性好等优点,在汽车领域常被用作保险杠、挡泥板、仪表盘等。随着新能源汽车和汽车轻量化目标的提出,对聚丙烯轻质化有了更高的要求,使用空心玻璃微珠填充改性聚丙烯,不仅可以降低聚丙烯密度,还能改善聚丙烯的流变性能。但是空心玻璃微珠是一种无机材料,与高分子有机物的相容性较差,直接将无机材料加入到基体塑料中,无机材料与基体塑料之间会形成间隙,会使塑料的力学性能大大降低。目前,改善二者之间相容性的方法有很多,但大多改善程度不足、稳定性差、性能单一。另外,聚丙烯的耐候老化性较差,氧指数较低需要改善,以满足汽车领域的更高需求。
发明内容
本发明的目的在于克服现有技术的缺陷,提供了一种空心玻璃微珠母粒的制备方法。
本发明的目的可以通过以下技术方案实现:
一种空心玻璃微珠母粒的制备方法,包括以下步骤:
A1、将空心玻璃微珠置于100℃下进行烘干处理,随后将干燥的微珠置于NaOH溶液(浓度为0.3mol/L)中,在60℃下搅拌4h,用去离子水和乙醇交替清洗3次,减压抽滤,除去多余的水分,置于烘干箱中100℃下烘干12h,得到预处理的空心玻璃微珠;
A2、将乙醇水溶液(乙醇与水的体积比为1:9)与γ-氨丙基三乙氧基硅烷(硅烷偶联剂KH-550)加入到三口烧瓶中,水解5min,然后加入预处理的空心玻璃微珠,在65℃的条件下搅拌4h,反应结束之后,减压抽滤,干燥,得到初步改性的空心玻璃微珠;
A3、将初步改性的空心玻璃微珠加入到吡啶中,磁力搅拌30min,加入改性剂和二月桂酸二丁基锡(催化剂),升温至80℃,保温反应6h,反应完成,减压蒸馏,干燥,得到改性空心玻璃微珠;
A4、将改性空心玻璃微珠、聚丙烯树脂、润滑剂、抗氧剂搅拌混合均匀,加入双螺杆挤出机中,熔融共混,挤出,造粒,得到空心玻璃微珠母粒。
进一步地,步骤A1中空心玻璃微珠、NaOH溶液的用量之比为100g:250mL。
进一步地,步骤A2中乙醇水溶液、硅烷偶联剂KH-550、预处理的空心玻璃微珠的用量之比为200mL:2g:100g。
进一步地,步骤A3中初步改性的空心玻璃微珠、吡啶、改性剂、二月桂酸二丁基锡的用量之比为100g:200mL:3g-9g:0.5g。
进一步地,步骤A4中润滑剂为PE蜡、硬脂酸镁、硬脂酸钙中的一种。
进一步地,步骤A4中抗氧剂为抗氧剂1010、抗氧剂1076中的一种。
进一步地,步骤A4中改性空心玻璃微珠、聚丙烯树脂、润滑剂、抗氧剂的质量之比为15:75:1:3。
将空心玻璃微珠进行预处理,能更好的与偶联剂发生反应;将改性剂接枝到空心玻璃微珠上,能大幅改善空心玻璃微珠与聚丙烯树脂的界面相容性,促进空心玻璃微珠均匀散,使空心玻璃微珠的性能得以充分发挥,并保证聚丙烯树脂的力学性能不受影响;另外,空心玻璃微珠属于无机填料,有机分子链通过接枝于其表面,难以渗出和迁移,使改性剂的性能可以长久保持。
进一步地,所述改性剂通过以下步骤制得:
S1、在装有搅拌装置的三口烧瓶中将2,2,6,6-四甲基哌啶醇、正辛烷、三氧化钼混合搅拌均匀,加热至85℃,滴加叔丁基过氧化氢水溶液,滴加完成后,回流反应10h,抽滤,滤液加入活性炭搅拌1h,静置,抽滤,取滤液,减压蒸馏除去正辛烷,得到中间体1;2,2,6,6-四甲基哌啶醇、正辛烷、三氧化钼、叔丁基过氧化氢水溶液的用量之比为15.7g:15.8g:0.4g:10.3g;
在三氧化钼的催化下和叔丁基过氧化氢的氧化下,2,2,6,6-四甲基哌啶醇与正辛烷发生自由基的偶联反应;正辛烷既作为反应物参与到反应过程中去,也作为反应溶剂,可以减少副产物的生成,得到中间体1;具体反应过程如下所示:
S2、在装有搅拌装置三口烧瓶中将中间体1、三氯氧磷、二丁基氧化锡(催化剂)、三乙胺和四氢呋喃混合搅拌均匀,然后缓慢升温至70℃,反应3h,反应完成,过滤除去三乙胺盐酸盐,减压蒸馏除去四氢呋喃,再通过柱层析提纯(洗脱液采用氯仿/乙醚的混合溶剂,二者的体积比为4:3),旋蒸除去洗脱液,得到中间体2;中间体1、三氯氧磷、二丁基氧化锡、三乙胺、四氢呋喃的用量之比为28.5g:18.2g:0.2g:50mL:100mL;
在二丁基氧化锡的催化剂下,中间体1与三氯氧磷发生酯化反应,通过控制二者的摩尔比接近1:1且三氯氧磷略微过量,使三氯氧磷上只有一个-Cl参与到反应,三乙胺除去反应生成的氯化氢,得到中间体2;具体反应过程如下所示:
S3、在装有搅拌回流装置三口烧瓶中充入氮气,将四甲基二乙烯基二硅氧烷、2-巯基乙醇、AIBN(偶氮二异丁腈)和乙腈搅拌混合均匀,于65℃下回流反应4h,反应完成,先旋蒸去除部分溶剂,再通过柱层析提纯(洗脱液采用乙醇/氯仿的混合溶剂,二者的体积比为4:1),旋蒸除去洗脱液,得到中间体3;四甲基二乙烯基二硅氧烷、2-巯基乙醇、AIBN、乙腈的用量之比为22.5g:7.8g:0.2g:50mL;
在偶氮二异丁腈作用下,四甲基二乙烯基二硅氧烷的端部不饱和碳碳双键与2-巯基乙醇发生巯基-烯的点击反应,通过控制二者的摩尔比接近1:1且四甲基二乙烯基二硅氧烷略微过量,使四甲基二乙烯基二硅氧烷上只有一个双键参与到反应,得到中间体3;反应过程如下所示:
S4、在装有搅拌装置三口烧瓶中将中间体2、中间体3、二月桂酸二丁基锡(催化剂)、三乙胺和四氢呋喃混合搅拌均匀,然后缓慢升温至80℃,反应6h,反应完成,过滤除去三乙胺盐酸盐,旋蒸去除部分溶剂,再通过柱层析提纯(洗脱液采用氯仿/乙醚的混合溶剂,二者的体积比为6:5),旋蒸除去洗脱液,得到改性剂;中间体2、中间体3、二月桂酸二丁基锡、三乙胺、四氢呋喃的用量之比为40.1g:28.5g:0.3g:50mL:150mL;
在二月桂酸二丁基锡的催化剂下,中间体2与中间体3发生酯化反应,通过控制二者的摩尔比接近1:1且中间体2略微过量,使中间体2上只有一个氯基参与到反应,三乙胺除去反应生成的氯化氢,得到改性剂;具体反应过程如下所示:
制得改性剂一端含有碳碳双键,在聚合反应中能连接在聚丙烯分子链上,提升相容性,使改性剂性能得到充分发挥;另外,改性剂含有P-N阻燃成分、-Si-O-Si-链段、受阻胺和长碳链结构。其中P-N阻燃成分是一种优秀的无卤阻燃成分,具备磷系和氮系阻燃剂的协同阻燃效果,能够赋予聚丙烯环保且高效的阻燃性能;-Si-O-Si-链段属于较好的阻燃和抑烟成分,不仅能进一步提升聚丙烯的阻燃性能,还具有一定的抑烟效果;不仅如此,受阻胺起到光稳定剂的作用,在光防护中会分解二氧化氢产生稳定的氮氧自由基,这种化合物能非常有效地捕获光氧化降解中所产生的自由基,能有效地抑制基体的光氧化降解,并且在稳定条件下可以再生,赋予了聚丙烯稳定高效的光稳定性;最后,长碳链属于亚甲基链节,具有很好的柔韧性,能提升聚丙烯的抗冲击性能,并且还能穿插进聚丙烯分子链中,提高稳定性;
需要补充说明的是,选用的抗氧剂为受阻酚类抗氧剂,能与改性剂起协同作用,进一步加强了聚丙烯的耐候耐老化性能。
本发明的有益效果:1、本发明通过将改性剂接枝在空心玻璃微珠表面,并通过聚合反应连接在聚丙烯分子链上,不仅改善了空心玻璃微珠与聚丙烯的相容性,而且与直接添加改性剂相比,这种方法使改性剂不易迁移和渗出,保证了性能的长久性。
2、改性剂含有多种功能基团,能显著提升聚丙烯母料的阻燃性能、耐候耐老化性能和一定程度的抗冲性能。
3、经空心玻璃微珠改性后的聚丙烯力学性能并未下降,并且密度较低,符合轻质化汽车领域的应用需求。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
实施例1
制备改性剂:
S1、在装有搅拌装置的三口烧瓶中将15.7g的2,2,6,6-四甲基哌啶醇、15.8g正辛烷、0.4g三氧化钼混合搅拌均匀,加热至85℃,滴加10.3g叔丁基过氧化氢水溶液(质量分数70%),滴加完成后,回流反应10h,抽滤,滤液加入活性炭搅拌1h,静置,抽滤,取滤液,减压蒸馏除去正辛烷,得到中间体1;
S2、在装有搅拌装置三口烧瓶中将28.5g中间体1、18.2g三氯氧磷、0.2g二丁基氧化锡、50mL三乙胺和100mL四氢呋喃混合搅拌均匀,然后缓慢升温至70℃,反应3h,反应完成,过滤,减压蒸馏除去四氢呋喃,再通过柱层析提纯(洗脱液采用氯仿/乙醚的混合溶剂,二者的体积比为4:3),旋蒸除去洗脱液,得到中间体2;
S3、在装有搅拌回流装置三口烧瓶中充入氮气,将22.5g四甲基二乙烯基二硅氧烷、7.8g的2-巯基乙醇、0.2g的AIBN和50mL乙腈搅拌混合均匀,于65℃下回流反应4h,反应完成,先旋蒸去除部分溶剂,再通过柱层析提纯(洗脱液采用乙醇/氯仿的混合溶剂,二者的体积比为4:1),旋蒸除去洗脱液,得到中间体3;
S4、在装有搅拌装置三口烧瓶中将40.1g中间体2、28.5g中间体3、0.3g二月桂酸二丁基锡、50mL三乙胺和150mL四氢呋喃混合搅拌均匀,然后缓慢升温至80℃,反应6h,反应完成,过滤,旋蒸去除部分溶剂,再通过柱层析提纯(洗脱液采用氯仿/乙醚的混合溶剂,二者的体积比为6:5),旋蒸除去洗脱液,得到改性剂。
实施例2
制备改性剂:
S1、在装有搅拌装置的三口烧瓶中将31.4g的2,2,6,6-四甲基哌啶醇、31.6g正辛烷、0.8g三氧化钼混合搅拌均匀,加热至85℃,滴加20.6g叔丁基过氧化氢水溶液(质量分数70%),滴加完成后,回流反应10h,抽滤,滤液加入活性炭搅拌1h,静置,抽滤,取滤液,减压蒸馏除去正辛烷,得到中间体1;
S2、在装有搅拌装置三口烧瓶中将57g中间体1、36.4g三氯氧磷、0.4g二丁基氧化锡、100mL三乙胺和200mL四氢呋喃混合搅拌均匀,然后缓慢升温至70℃,反应3h,反应完成,过滤,减压蒸馏除去四氢呋喃,再通过柱层析提纯(洗脱液采用氯仿/乙醚的混合溶剂,二者的体积比为4:3),旋蒸除去洗脱液,得到中间体2;
S3、在装有搅拌回流装置三口烧瓶中充入氮气,将45g四甲基二乙烯基二硅氧烷、15.6g的2-巯基乙醇、0.4g的AIBN和100mL乙腈搅拌混合均匀,于65℃下回流反应4h,反应完成,先旋蒸去除部分溶剂,再通过柱层析提纯(洗脱液采用乙醇/氯仿的混合溶剂,二者的体积比为4:1),旋蒸除去洗脱液,得到中间体3;
S4、在装有搅拌装置三口烧瓶中将80.2g中间体2、57g中间体3、0.6g二月桂酸二丁基锡、100mL三乙胺和300mL四氢呋喃混合搅拌均匀,然后缓慢升温至80℃,反应6h,反应完成,过滤,旋蒸去除部分溶剂,再通过柱层析提纯(洗脱液采用氯仿/乙醚的混合溶剂,二者的体积比为6:5),旋蒸除去洗脱液,得到改性剂。
实施例3
A1、将100g空心玻璃微珠置于100℃下进行烘干处理,随后将干燥的微珠置于250mL的NaOH溶液(浓度为0.3mol/L)中,在60℃下搅拌4h,用去离子水和乙醇交替清洗3次,减压抽滤,除去多余的水分,置于烘干箱中100℃下烘干12h,得到预处理的空心玻璃微珠;
A2、将200mL乙醇水溶液(乙醇与水的体积比为1:9)与2g硅烷偶联剂KH-550加入到三口烧瓶中,水解5min,然后加入100g预处理的空心玻璃微珠,在65℃的条件下搅拌4h,反应结束之后,减压抽滤,干燥,得到初步改性的空心玻璃微珠;
A3、将100g初步改性的空心玻璃微珠加入到200mL吡啶中,磁力搅拌30min,加入3g由实施例1制得的改性剂和0.5g二月桂酸二丁基锡,升温至80℃,保温反应6h,反应完成,减压蒸馏,干燥,得到改性空心玻璃微珠;
A4、将15g改性空心玻璃微珠、75g聚丙烯树脂、1gPE蜡、3g抗氧剂1076搅拌混合均匀,加入双螺杆挤出机中,熔融共混,挤出,造粒,得到空心玻璃微珠母粒。
实施例4
A1、将100g空心玻璃微珠置于100℃下进行烘干处理,随后将干燥的微珠置于250mL的NaOH溶液(浓度为0.3mol/L)中,在60℃下搅拌4h,用去离子水和乙醇交替清洗3次,减压抽滤,除去多余的水分,置于烘干箱中100℃下烘干12h,得到预处理的空心玻璃微珠;
A2、将200mL乙醇水溶液(乙醇与水的体积比为1:9)与2g硅烷偶联剂KH-550加入到三口烧瓶中,水解5min,然后加入100g预处理的空心玻璃微珠,在65℃的条件下搅拌4h,反应结束之后,减压抽滤,干燥,得到初步改性的空心玻璃微珠;
A3、将100g初步改性的空心玻璃微珠加入到200mL吡啶中,磁力搅拌30min,加入6g由实施例2制得的改性剂和0.5g二月桂酸二丁基锡,升温至80℃,保温反应6h,反应完成,减压蒸馏,干燥,得到改性空心玻璃微珠;
A4、将15g改性空心玻璃微珠、75g聚丙烯树脂、1g硬脂酸镁、3g抗氧剂1010搅拌混合均匀,加入双螺杆挤出机中,熔融共混,挤出,造粒,得到空心玻璃微珠母粒。
实施例5
A1、将100g空心玻璃微珠置于100℃下进行烘干处理,随后将干燥的微珠置于250mL的NaOH溶液(浓度为0.3mol/L)中,在60℃下搅拌4h,用去离子水和乙醇交替清洗3次,减压抽滤,除去多余的水分,置于烘干箱中100℃下烘干12h,得到预处理的空心玻璃微珠;
A2、将200mL乙醇水溶液(乙醇与水的体积比为1:9)与2g硅烷偶联剂KH-550加入到三口烧瓶中,水解5min,然后加入100g预处理的空心玻璃微珠,在65℃的条件下搅拌4h,反应结束之后,减压抽滤,干燥,得到初步改性的空心玻璃微珠;
A3、将100g初步改性的空心玻璃微珠加入到200mL吡啶中,磁力搅拌30min,加入9g由实施例2制得的改性剂和0.5g二月桂酸二丁基锡,升温至80℃,保温反应6h,反应完成,减压蒸馏,干燥,得到改性空心玻璃微珠;
A4、将15g改性空心玻璃微珠、75g聚丙烯树脂、1g硬脂酸钙、3g抗氧剂1010搅拌混合均匀,加入双螺杆挤出机中,熔融共混,挤出,造粒,得到空心玻璃微珠母粒。
对比例1
与实施例5不同的是,步骤A3中不加入助剂。
对比例2
使用市售东莞市星原化工有限公司生产的PP玻璃微珠母粒。
将实施例3-5,对比例1-2根据不同测试标准制成相应形状,进行如下的性能测试:
采用国家标准GB/T 1033.1-2008《塑料 非泡沫塑料密度的测定》测定密度;
采用国家标准GB/T 2406-2008《塑料燃烧性能试验方法》测定极限氧指数;
采用国家标准GB/T 1040.2-2006《塑料 拉伸性能的测定》测定拉伸强度;
采用国家标准GB/T 1843-2008《塑料悬臂梁冲击强度的测定》测定冲击强度;
采用国家标准GB/T 16422.2-2014《塑料 实验室光源暴露试验方法》将试样暴露在氙弧灯下,测定试样试验前后的表面光泽,并计算光泽保持率;光泽保持率=试验后光泽/试验前光泽,光泽保持率越高,其耐候性能越好。
测得结果如下表所示:
由上表可知,实施例3-5随着改性剂的用量不断增加,母料的各项性能都有所提升,因此,制得的母粒具有稳定高效的阻燃性能、耐候耐老化性能,并且力学强度高,密度低,质轻,在轻质化汽车领域具备重要应用价值。
在说明书的描述中,参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不一定指的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上内容仅仅是对本发明所作的举例和说明,所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代,只要不偏离发明或者超越本权利要求书所定义的范围,均应属于本发明的保护范围。
Claims (7)
1.一种空心玻璃微珠母粒的制备方法,其特征在于,包括以下步骤:
A1、将空心玻璃微珠置于100℃下进行烘干,将干燥的微珠置于NaOH溶液中,在60℃下搅拌4h,用去离子水和乙醇交替清洗3次,减压抽滤,置于烘干箱中100℃下烘干12h,得到预处理的空心玻璃微珠;
A2、将乙醇水溶液与硅烷偶联剂KH-550加入到三口烧瓶中,水解5min,加入预处理的空心玻璃微珠,在65℃的条件下搅拌4h,减压抽滤,干燥,得到初步改性的空心玻璃微珠;
A3、将初步改性的空心玻璃微珠加入到吡啶中,磁力搅拌30min,加入改性剂和二月桂酸二丁基锡,升温至80℃,保温反应6h,减压蒸馏,干燥,得到改性空心玻璃微珠;
A4、将改性空心玻璃微珠、聚丙烯树脂、润滑剂、抗氧剂搅拌混合均匀,加入双螺杆挤出机中,熔融共混,挤出造粒,得到空心玻璃微珠母粒;
其中改性剂通过以下步骤制得:
S1、将2,2,6,6-四甲基哌啶醇、正辛烷、三氧化钼混合搅拌均匀,加热至85℃,滴加叔丁基过氧化氢水溶液,回流反应10h,抽滤,滤液加入活性炭搅拌1h,静置,抽滤,取滤液,减压蒸馏,得到中间体1;
S2、将中间体1、三氯氧磷、二丁基氧化锡、三乙胺和四氢呋喃混合搅拌均匀,然后缓慢升温至70℃,反应3h,过滤除去三乙胺盐酸盐,减压蒸馏,柱层析提纯,旋蒸,得到中间体2;
S3、在三口烧瓶中充入氮气,将四甲基二乙烯基二硅氧烷、2-巯基乙醇、AIBN和乙腈搅拌混合均匀,于65℃下回流反应4h,先旋蒸,柱层析提纯,旋蒸,得到中间体3;
S4、在三口烧瓶中将中间体2、中间体3、二月桂酸二丁基锡、三乙胺和四氢呋喃混合搅拌均匀,然后缓慢升温至80℃,反应6h,过滤,旋蒸,柱层析提纯,旋蒸,得到改性剂。
2.根据权利要求1所述的一种空心玻璃微珠母粒的制备方法,其特征在于,步骤A3中初步改性的空心玻璃微珠、吡啶、改性剂、二月桂酸二丁基锡的用量之比为100g:200mL:3g-9g:0.5g。
3.根据权利要求1所述的一种空心玻璃微珠母粒的制备方法,其特征在于,步骤A4中改性空心玻璃微珠、聚丙烯树脂、润滑剂、抗氧剂的质量之比为15:75:1:3。
4.根据权利要求1所述的一种空心玻璃微珠母粒的制备方法,其特征在于,步骤S1中2,2,6,6-四甲基哌啶醇、正辛烷、三氧化钼、叔丁基过氧化氢水溶液的用量之比为15.7g:15.8g:0.4g:10.3g。
5.根据权利要求1所述的一种空心玻璃微珠母粒的制备方法,其特征在于,步骤S2中中间体1、三氯氧磷、二丁基氧化锡、三乙胺、四氢呋喃的用量之比为28.5g:18.2g:0.2g:50mL:100mL。
6.根据权利要求1所述的一种空心玻璃微珠母粒的制备方法,其特征在于,步骤S3中四甲基二乙烯基二硅氧烷、2-巯基乙醇、AIBN、乙腈的用量之比为22.5g:7.8g:0.2g:50mL。
7.根据权利要求1所述的一种空心玻璃微珠母粒的制备方法,其特征在于,步骤S4中中间体2、中间体3、二月桂酸二丁基锡、三乙胺、四氢呋喃的用量之比为40.1g:28.5g:0.3g:50mL:150mL。
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