CN116804130A - 一种低voc的tpo汽车内饰材料及其生产工艺 - Google Patents
一种低voc的tpo汽车内饰材料及其生产工艺 Download PDFInfo
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- CN116804130A CN116804130A CN202310494330.XA CN202310494330A CN116804130A CN 116804130 A CN116804130 A CN 116804130A CN 202310494330 A CN202310494330 A CN 202310494330A CN 116804130 A CN116804130 A CN 116804130A
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 32
- 239000008367 deionised water Substances 0.000 claims abstract description 26
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- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 21
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- 239000002344 surface layer Substances 0.000 claims abstract description 12
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- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 70
- 238000003756 stirring Methods 0.000 claims description 65
- 238000006243 chemical reaction Methods 0.000 claims description 44
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 35
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 33
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims description 32
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 30
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 30
- KDXKERNSBIXSRK-YFKPBYRVSA-N L-lysine Chemical compound NCCCC[C@H](N)C(O)=O KDXKERNSBIXSRK-YFKPBYRVSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000002904 solvent Substances 0.000 claims description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 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 20
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 20
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 20
- 238000002390 rotary evaporation Methods 0.000 claims description 20
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 20
- YIHRGKXNJGKSOT-UHFFFAOYSA-N 1,1,2,2,3,3-hexafluorobutan-1-ol Chemical compound CC(F)(F)C(F)(F)C(O)(F)F YIHRGKXNJGKSOT-UHFFFAOYSA-N 0.000 claims description 16
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 16
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 15
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 14
- 239000011248 coating agent Substances 0.000 claims description 13
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- 235000019766 L-Lysine Nutrition 0.000 claims description 12
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- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 claims description 11
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 11
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 11
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 10
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- 238000001035 drying Methods 0.000 claims description 10
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- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
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- 229920001451 polypropylene glycol Polymers 0.000 claims description 10
- 235000021355 Stearic acid Nutrition 0.000 claims description 9
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- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 9
- 239000008117 stearic acid Substances 0.000 claims description 9
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- 239000012044 organic layer Substances 0.000 claims description 7
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- 239000000203 mixture Substances 0.000 claims description 6
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 5
- 239000004698 Polyethylene Substances 0.000 claims description 5
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- 239000004595 color masterbatch Substances 0.000 claims description 5
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- 239000000839 emulsion Substances 0.000 claims description 5
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- BCDGQXUMWHRQCB-UHFFFAOYSA-N glycine methyl ketone Natural products CC(=O)CN BCDGQXUMWHRQCB-UHFFFAOYSA-N 0.000 claims description 5
- 239000005457 ice water Substances 0.000 claims description 5
- 239000004611 light stabiliser Substances 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 229920000573 polyethylene Polymers 0.000 claims description 5
- 229920001155 polypropylene Polymers 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 238000010025 steaming Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000012752 auxiliary agent Substances 0.000 claims description 2
- 238000013329 compounding Methods 0.000 claims description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 2
- 230000037452 priming Effects 0.000 claims 1
- 239000012855 volatile organic compound Substances 0.000 description 20
- GJKGAPPUXSSCFI-UHFFFAOYSA-N 2-Hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone Chemical compound CC(C)(O)C(=O)C1=CC=C(OCCO)C=C1 GJKGAPPUXSSCFI-UHFFFAOYSA-N 0.000 description 6
- 229910052731 fluorine Inorganic materials 0.000 description 5
- 239000011737 fluorine Substances 0.000 description 5
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 4
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 4
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 4
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- 150000002009 diols Chemical class 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 2
- 238000000016 photochemical curing Methods 0.000 description 2
- 229920006124 polyolefin elastomer Polymers 0.000 description 2
- 239000004970 Chain extender Substances 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 150000001263 acyl chlorides Chemical class 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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- C—CHEMISTRY; METALLURGY
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
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- C08G18/3206—Polyhydroxy compounds aliphatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3225—Polyamines
- C08G18/3228—Polyamines acyclic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/348—Hydroxycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
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- C08G18/6692—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/34
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/677—Low-molecular-weight compounds containing heteroatoms other than oxygen and the nitrogen of primary or secondary amino groups
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- C09D5/002—Priming paints
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- 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
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- C08K3/24—Acids; Salts thereof
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- C08K2003/265—Calcium, strontium or barium carbonate
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
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- Inorganic Chemistry (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
本发明公开了一种低VOC的TPO汽车内饰材料及其生产工艺,从下往上依次为聚烯烃海绵层、TPO表层和水漆层,所述水汽层包括水性底漆层和水性面漆层,其特征在于:所述水性底漆层包括如下重量份原料:75‑100份改性聚氨酯,0.1‑0.8份消泡剂,0.3‑0.5份分散剂,5‑10份纳米碳酸钙,2‑5份硅溶胶,1.2‑2.0份光引发剂,30‑50份去离子水;在TPO材料涂覆水性聚氨酯漆,一方面能够降低VOC排放,另一方面能够提高漆面层的疏水性能。
Description
技术领域
本发明涉及汽车内饰材料技术领域,具体涉及一种低VOC的TPO汽车内饰材料及其生产工艺。
背景技术
热塑性聚烯烃弹性体(TPO)主要由橡胶和聚烯烃两种组分组成,具有高弹性、高强度、高伸长率和良好的低温性能,又具有优异的耐热耐老化和抗紫外性能,在常温下成橡胶弹性,密度小、弯曲大、低温抗冲击性能高、易加工、可重复使用等优点,广泛应用于汽车部件、电子电气、建筑密封、运动器械、机械行业等领域。
聚烯烃弹性体材料表面通常需要进行涂饰一层油漆,用来提高抗刮擦性能以及提供良好手感;但目前应用在聚烯烃弹性体表面的油漆通常为溶剂型聚氨酯油漆,常以甲苯,丁酮等等材料作为溶剂,而产品残留的溶剂会导致VOC的超标。
发明内容
为了解决上述技术问题,本发明提供一种低VOC的TPO汽车内饰材料及其生产工艺。
本发明的目的可以通过以下技术方案实现:
一种低VOC的TPO汽车内饰材料,从下往上依次为聚烯烃海绵层、TPO表层和水漆层,所述水汽层包括水性底漆层和水性面漆层,所述水性底漆层包括如下重量份原料:75-100份改性聚氨酯,0.1-0.8份消泡剂(IOTA 1810),0.3-0.5份分散剂(十二烷基硫酸钠、聚丙烯酸钠或硬脂酸),5-10份纳米碳酸钙,2-5份硅溶胶,1.2-2.0份光引发剂(2959),30-50份去离子水;
所述水性面漆层包括如下重量份原料:75-100份改性聚氨酯,0.1-0.8份消泡剂(IOTA 1810),0.3-0.5份分散剂(十二烷基硫酸钠、聚丙烯酸钠或硬脂酸),2-5份硅溶胶,1.2-2.0份光引发剂(2959),30-50份去离子水;
所述改性聚氨酯包括如下步骤制成:
将聚丙二醇、1,4-丁二醇、二羟甲基丙酸和二元醇加入三口烧瓶中,通入氮气,升温至80℃以200r/min的转速磁力搅拌2h,加入异佛尔酮二异氰酸酯和二月桂酸二丁基锡,保温反应3h,反应结束后加入丙酮和三乙胺,搅拌30min,之后以1000r/min的转速匀速搅拌并加入去离子水和乙二胺,搅拌1h,制得乳液,在温度50℃下、真空度0.09MPa下除去丙酮,制得改性聚氨酯。
进一步地,所述聚丙二醇、1,4-丁二醇、二羟甲基丙酸、异佛尔酮二异氰酸酯、三乙胺、乙二胺和二元醇的用量比为20g∶4.10-4.12g∶2.02-2.06g∶22.23g∶1.57-1.60g∶1g∶4.24-4.32g,二月桂酸二丁基锡的用量为单体重量和的3-5%。
进一步地,所述二元醇包括如下步骤制成:
步骤S1、将六氟正丁醇加入装有丙酮的三口烧瓶中,通入氮气,升温至80℃,在200r/min的转速下匀速搅拌并加入L-赖氨酸三异氰酸酯和二月桂酸二丁基锡,匀速搅拌并保温反应3h,反应结束后降温至室温,加入二乙醇胺,继续搅拌并反应20min,旋蒸除去溶剂,制得中间体1;
步骤S1中六氟正丁醇上的醇羟基先和L-赖氨酸三异氰酸酯上的一个异氰酸酯基反应,之后降温至室温,L-赖氨酸三异氰酸酯上的第二个异氰酸酯与二乙醇胺上的仲胺反应,生成中间体1,其为一种含有氟键的二元醇;
步骤S2、将衣康酸和丙烯酸羟乙酯加入装有甲苯的四口烧瓶中,升温至60℃,氮气气氛下加入对甲苯磺酸,匀速搅拌并反应4h,反应结束后升温至70℃,继续搅拌并反应30min,反应结束后用无水硫酸镁除去水,蒸出溶剂,在40℃下抽真空4h,制得中间体2;
步骤S2中衣康酸上的一个羧基和丙烯酸羟乙酯上的一个羟基反应,生成中间体2,结构如下所示,该结构中引入了衣康酸结构,引入了不饱和的碳碳双键,
步骤S3、将中间体2加入三口烧瓶中,之后加入二氯亚砜,回流反应12h,反应结束后旋蒸除去剩余二氯亚砜,制得滤饼,之后加入四氢呋喃中,过滤,旋蒸除去溶剂,制得中间体3;
步骤S3中通过二氯亚砜合成中间体3,在中间体3的结构中引入酰氯,中间体3结构如下所示:
步骤S4、将中间体3加入四氢呋喃中,冰水浴下缓慢滴加至浓氨水中,室温下匀速搅拌24h,反应结束后减压蒸出四氢呋喃,用二氯甲烷萃取三次,有机层洗涤后干燥、重结晶,之后将制得的化合物采用霍夫曼降解反应制成中间体4;
步骤S4中中间体3与浓氨水反应,形成酰胺,之后采用霍夫曼降解反应制成中间体4,在中间体4结构中引入了氨基,过程如下所示:
步骤S5、将中间体4和中间体1加入四氢呋喃中,室温下匀速搅拌并反应30-45min,旋蒸除去溶剂,制得二元醇,控制中间体4和中间体1的摩尔比为1∶1。
步骤S5中中间体4上的氨基与中间体1上的剩余的一个异氰酸酯基反应,制成出二元醇,其为一种端羟基含氟含衣康酸以及碳碳双键的二元醇。
进一步地:步骤S1中控制六氟正丁醇、L-赖氨酸三异氰酸酯和二乙醇胺的摩尔比为1∶1∶1,二月桂酸二丁基锡的用量为六氟正丁醇重量的1-2%,步骤S2中控制衣康酸、丙烯酸羟乙酯、对甲苯磺酸和甲苯的用量比为0.1mol∶0.1mol∶0.02g∶20mL,步骤S3中控制中间体2和二氯亚砜的摩尔比为0.1-0.2mol∶0.4-0.5mol,步骤S4中控制中间体3、浓氨水和四氢呋喃的用量比为0.1mol∶200mL∶50mL。
一种低VOC的TPO汽车内饰材料的生产工艺,包括如下步骤:
第一步、按重量份计,将20-50份半交联TPO、10-30份聚丙烯、10-30份聚乙烯、1-3份光稳定剂(UV-119)、10-20份纳米碳酸钙、10-15份硬脂酸类助剂和5-10份色母粒混合均匀后加入挤出机中,挤出后形成TPO薄膜,电晕处理后制得TPO表层;
第二步、将改性聚氨酯、纳米碳酸钙、硅溶胶、光引发剂和去离子水混合均匀后加入消泡剂和分散剂,搅拌均匀,制得水性底漆;
第三步、将改性聚氨酯、硅溶胶、光引发剂和去离子水混合均匀后加入消泡剂和分散剂,搅拌均匀,制得水性面漆;
第四步、在TPO一侧表面涂覆水性底漆,在紫外光(1kW,800mJ/cm2)照下照射30s,形成水性面漆层,之后涂覆水性面漆,在紫外光照下照射30s,固化后形成水性面漆层,烘干,之后在TPO另一侧表面复合聚烯烃海绵,制得低VOC的TPO汽车内饰材料。
本发明的有益效果:
本发明制备出一种低VOC的TPO汽车内饰材料,在TPO材料涂覆水性聚氨酯漆,一方面能够降低VOC排放,另一方面能够提高漆面层的疏水性能;其中水性聚氨酯漆由改性聚氨酯基体制成,改性聚氨酯在合成过程中引入了亲水的二羟甲基丙酸单体和合成的二元醇,通过引入亲水单体制成水性漆,不用使用有机溶剂,能够降低VOC,而二元醇为一种端羟基含氟含衣康酸以及碳碳双键的二元醇,将其作为扩链剂引入聚氨酯硬段上,含氟链段能够提高聚氨酯漆面的疏水性能,而且引入的衣康酸结构和不饱和双键能够赋予光固化性能,使得合成出的水性漆同时兼具水性涂料和光固化的优点。
具体实施方式
下面将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
所述水性底漆层包括如下重量份原料:75份改性聚氨酯,0.1份消泡剂IOTA 1810,0.3份分散剂聚丙烯酸钠,5份纳米碳酸钙,2份硅溶胶,1.2份光引发剂2959,30份去离子水;
所述水性面漆层包括如下重量份原料:75份改性聚氨酯,0.1份消泡剂IOTA 1810,0.3份分散剂聚丙烯酸钠,2份硅溶胶,1.2份光引发剂2959,30份去离子水;
所述改性聚氨酯包括如下步骤制成:
将聚丙二醇、1,4-丁二醇、二羟甲基丙酸和二元醇加入三口烧瓶中,通入氮气,升温至80℃以200r/min的转速磁力搅拌2h,加入异佛尔酮二异氰酸酯和二月桂酸二丁基锡,保温反应3h,反应结束后加入丙酮和三乙胺,搅拌30min,之后以1000r/min的转速匀速搅拌并加入去离子水和乙二胺,搅拌1h,制得乳液,在温度50℃下、真空度0.09MPa下除去丙酮,制得改性聚氨酯,所述聚丙二醇、1,4-丁二醇、二羟甲基丙酸、异佛尔酮二异氰酸酯、三乙胺、乙二胺和二元醇的用量比为20g∶4.10g∶2.02g∶22.23g∶1.57g∶1g∶4.24g,二月桂酸二丁基锡的用量为单体重量和的3%。
所述二元醇包括如下步骤制成:
步骤S1、将六氟正丁醇加入装有丙酮的三口烧瓶中,通入氮气,升温至80℃,在200r/min的转速下匀速搅拌并加入L-赖氨酸三异氰酸酯和二月桂酸二丁基锡,匀速搅拌并保温反应3h,反应结束后降温至室温,加入二乙醇胺,继续搅拌并反应20min,旋蒸除去溶剂,制得中间体1,控制六氟正丁醇、L-赖氨酸三异氰酸酯和二乙醇胺的摩尔比为1∶1∶1,二月桂酸二丁基锡的用量为六氟正丁醇重量的1%;
步骤S2、将衣康酸和丙烯酸羟乙酯加入装有甲苯的四口烧瓶中,升温至60℃,氮气气氛下加入对甲苯磺酸,匀速搅拌并反应4h,反应结束后升温至70℃,继续搅拌并反应30min,反应结束后用无水硫酸镁除去水,蒸出溶剂,在40℃下抽真空4h,制得中间体2,控制衣康酸、丙烯酸羟乙酯、对甲苯磺酸和甲苯的用量比为0.1mol∶0.1mol∶0.02g∶20mL;
步骤S3、将中间体2加入三口烧瓶中,之后加入二氯亚砜,回流反应12h,反应结束后旋蒸除去剩余二氯亚砜,制得滤饼,之后加入四氢呋喃中,过滤,旋蒸除去溶剂,制得中间体3,控制中间体2和二氯亚砜的摩尔比为0.1mol∶0.4mol;
步骤S4、将中间体3加入四氢呋喃中,冰水浴下缓慢滴加至浓氨水中,室温下匀速搅拌24h,反应结束后减压蒸出四氢呋喃,用二氯甲烷萃取三次,有机层洗涤后干燥、重结晶,之后将制得的化合物采用霍夫曼降解反应制成中间体4,控制中间体3、浓氨水和四氢呋喃的用量比为0.1mol∶200mL∶50mL;
步骤S5、将中间体4和中间体1加入四氢呋喃中,室温下匀速搅拌并反应30min,旋蒸除去溶剂,制得二元醇,控制中间体4和中间体1的摩尔比为1∶1。
实施例2
所述水性底漆层包括如下重量份原料:85份改性聚氨酯,0.3份消泡剂IOTA 1810,0.4份分散剂十二烷基硫酸钠,8份纳米碳酸钙,4份硅溶胶,1.5份光引发剂2959,40份去离子水;
所述水性面漆层包括如下重量份原料:85份改性聚氨酯,0.3份消泡剂IOTA 1810,0.4份分散剂十二烷基硫酸钠,4份硅溶胶,1.5份光引发剂2959,40份去离子水;
所述改性聚氨酯包括如下步骤制成:
将聚丙二醇、1,4-丁二醇、二羟甲基丙酸和二元醇加入三口烧瓶中,通入氮气,升温至80℃以200r/min的转速磁力搅拌2h,加入异佛尔酮二异氰酸酯和二月桂酸二丁基锡,保温反应3h,反应结束后加入丙酮和三乙胺,搅拌30min,之后以1000r/min的转速匀速搅拌并加入去离子水和乙二胺,搅拌1h,制得乳液,在温度50℃下、真空度0.09MPa下除去丙酮,制得改性聚氨酯,所述聚丙二醇、1,4-丁二醇、二羟甲基丙酸、异佛尔酮二异氰酸酯、三乙胺、乙二胺和二元醇的用量比为20g∶4.11g∶2.04g∶22.23g∶1.58g∶1g∶4.30g,二月桂酸二丁基锡的用量为单体重量和的4%。
所述二元醇包括如下步骤制成:
步骤S1、将六氟正丁醇加入装有丙酮的三口烧瓶中,通入氮气,升温至80℃,在200r/min的转速下匀速搅拌并加入L-赖氨酸三异氰酸酯和二月桂酸二丁基锡,匀速搅拌并保温反应3h,反应结束后降温至室温,加入二乙醇胺,继续搅拌并反应20min,旋蒸除去溶剂,制得中间体1,控制六氟正丁醇、L-赖氨酸三异氰酸酯和二乙醇胺的摩尔比为1∶1∶1,二月桂酸二丁基锡的用量为六氟正丁醇重量的1.5%;
步骤S2、将衣康酸和丙烯酸羟乙酯加入装有甲苯的四口烧瓶中,升温至60℃,氮气气氛下加入对甲苯磺酸,匀速搅拌并反应4h,反应结束后升温至70℃,继续搅拌并反应30min,反应结束后用无水硫酸镁除去水,蒸出溶剂,在40℃下抽真空4h,制得中间体2,控制衣康酸、丙烯酸羟乙酯、对甲苯磺酸和甲苯的用量比为0.1mol∶0.1mol∶0.02g∶20mL;
步骤S3、将中间体2加入三口烧瓶中,之后加入二氯亚砜,回流反应12h,反应结束后旋蒸除去剩余二氯亚砜,制得滤饼,之后加入四氢呋喃中,过滤,旋蒸除去溶剂,制得中间体3,控制中间体2和二氯亚砜的摩尔比为0.1mol∶0.5mol;
步骤S4、将中间体3加入四氢呋喃中,冰水浴下缓慢滴加至浓氨水中,室温下匀速搅拌24h,反应结束后减压蒸出四氢呋喃,用二氯甲烷萃取三次,有机层洗涤后干燥、重结晶,之后将制得的化合物采用霍夫曼降解反应制成中间体4,控制中间体3、浓氨水和四氢呋喃的用量比为0.1mol∶200mL∶50mL;
步骤S5、将中间体4和中间体1加入四氢呋喃中,室温下匀速搅拌并反应45min,旋蒸除去溶剂,制得二元醇,控制中间体4和中间体1的摩尔比为1∶1。
实施例3
所述水性底漆层包括如下重量份原料:100份改性聚氨酯,0.8份消泡剂IOTA1810,0.5份分散剂硬脂酸,10份纳米碳酸钙,5份硅溶胶,2.0份光引发剂2959,50份去离子水;
所述水性面漆层包括如下重量份原料:100份改性聚氨酯,0.8份消泡剂IOTA1810,0.5份分散剂硬脂酸,5份硅溶胶,2.0份光引发剂2959,50份去离子水;
所述改性聚氨酯包括如下步骤制成:
将聚丙二醇、1,4-丁二醇、二羟甲基丙酸和二元醇加入三口烧瓶中,通入氮气,升温至80℃以200r/min的转速磁力搅拌2h,加入异佛尔酮二异氰酸酯和二月桂酸二丁基锡,保温反应3h,反应结束后加入丙酮和三乙胺,搅拌30min,之后以1000r/min的转速匀速搅拌并加入去离子水和乙二胺,搅拌1h,制得乳液,在温度50℃下、真空度0.09MPa下除去丙酮,制得改性聚氨酯,所述聚丙二醇、1,4-丁二醇、二羟甲基丙酸、异佛尔酮二异氰酸酯、三乙胺、乙二胺和二元醇的用量比为20g∶4.12g∶2.06g∶22.23g∶1.60g∶1g∶4.32g,二月桂酸二丁基锡的用量为单体重量和的5%。
所述二元醇包括如下步骤制成:
步骤S1、将六氟正丁醇加入装有丙酮的三口烧瓶中,通入氮气,升温至80℃,在200r/min的转速下匀速搅拌并加入L-赖氨酸三异氰酸酯和二月桂酸二丁基锡,匀速搅拌并保温反应3h,反应结束后降温至室温,加入二乙醇胺,继续搅拌并反应20min,旋蒸除去溶剂,制得中间体1,控制六氟正丁醇、L-赖氨酸三异氰酸酯和二乙醇胺的摩尔比为1∶1∶1,二月桂酸二丁基锡的用量为六氟正丁醇重量的2%;
步骤S2、将衣康酸和丙烯酸羟乙酯加入装有甲苯的四口烧瓶中,升温至60℃,氮气气氛下加入对甲苯磺酸,匀速搅拌并反应4h,反应结束后升温至70℃,继续搅拌并反应30min,反应结束后用无水硫酸镁除去水,蒸出溶剂,在40℃下抽真空4h,制得中间体2,控制衣康酸、丙烯酸羟乙酯、对甲苯磺酸和甲苯的用量比为0.1mol∶0.1mol∶0.02g∶20mL;
步骤S3、将中间体2加入三口烧瓶中,之后加入二氯亚砜,回流反应12h,反应结束后旋蒸除去剩余二氯亚砜,制得滤饼,之后加入四氢呋喃中,过滤,旋蒸除去溶剂,制得中间体3,控制中间体2和二氯亚砜的摩尔比为0.2mol∶0.5mol;
步骤S4、将中间体3加入四氢呋喃中,冰水浴下缓慢滴加至浓氨水中,室温下匀速搅拌24h,反应结束后减压蒸出四氢呋喃,用二氯甲烷萃取三次,有机层洗涤后干燥、重结晶,之后将制得的化合物采用霍夫曼降解反应制成中间体4,控制中间体3、浓氨水和四氢呋喃的用量比为0.1mol∶200mL∶50mL;
步骤S5、将中间体4和中间体1加入四氢呋喃中,室温下匀速搅拌并反应30-45min,旋蒸除去溶剂,制得二元醇,控制中间体4和中间体1的摩尔比为1∶1。
实施例4
一种低VOC的TPO汽车内饰材料,从下往上依次为聚烯烃海绵层、TPO表层和水漆层,所述水汽层包括水性底漆层和水性面漆层;
该汽车内饰材料的生产工艺,包括如下步骤:
第一步、按重量份计,将20份半交联TPO、10份聚丙烯、10份聚乙烯、1份光稳定剂UV-119、10份纳米碳酸钙、10份硬脂酸和5份色母粒混合均匀后加入挤出机中,挤出后形成TPO薄膜,电晕处理后制得TPO表层;
第二步、将改性聚氨酯、纳米碳酸钙、硅溶胶、光引发剂和去离子水混合均匀后加入消泡剂和分散剂,搅拌均匀,制得水性底漆;
第三步、将改性聚氨酯、硅溶胶、光引发剂和去离子水混合均匀后加入消泡剂和分散剂,搅拌均匀,制得水性面漆;
第四步、在TPO一侧表面涂覆水性底漆,在紫外光1kW,800mJ/cm2下照射30s,形成水性面漆层,之后涂覆水性面漆,在紫外光照下照射30s,固化后形成水性面漆层,烘干,之后在TPO另一侧表面复合聚烯烃海绵,制得低VOC的TPO汽车内饰材料。
实施例5
一种低VOC的TPO汽车内饰材料,从下往上依次为聚烯烃海绵层、TPO表层和水漆层,所述水汽层包括水性底漆层和水性面漆层;
该汽车内饰材料的生产工艺,包括如下步骤:
第一步、按重量份计,将30份半交联TPO、20份聚丙烯、20份聚乙烯、2份光稳定剂UV-119、15份纳米碳酸钙、12份硬脂酸和8份色母粒混合均匀后加入挤出机中,挤出后形成TPO薄膜,电晕处理后制得TPO表层;
第二步、将改性聚氨酯、纳米碳酸钙、硅溶胶、光引发剂和去离子水混合均匀后加入消泡剂和分散剂,搅拌均匀,制得水性底漆;
第三步、将改性聚氨酯、硅溶胶、光引发剂和去离子水混合均匀后加入消泡剂和分散剂,搅拌均匀,制得水性面漆;
第四步、在TPO一侧表面涂覆水性底漆,在紫外光1kW,800mJ/cm2下照射30s,形成水性面漆层,之后涂覆水性面漆,在紫外光照下照射30s,固化后形成水性面漆层,烘干,之后在TPO另一侧表面复合聚烯烃海绵,制得低VOC的TPO汽车内饰材料。
实施例6
一种低VOC的TPO汽车内饰材料,从下往上依次为聚烯烃海绵层、TPO表层和水漆层,所述水汽层包括水性底漆层和水性面漆层;
该汽车内饰材料的生产工艺,包括如下步骤:
第一步、按重量份计,将50份半交联TPO、30份聚丙烯、30份聚乙烯、3份光稳定剂UV-119、20份纳米碳酸钙、15份硬脂酸和10份色母粒混合均匀后加入挤出机中,挤出后形成TPO薄膜,电晕处理后制得TPO表层;
第二步、将改性聚氨酯、纳米碳酸钙、硅溶胶、光引发剂和去离子水混合均匀后加入消泡剂和分散剂,搅拌均匀,制得水性底漆;
第三步、将改性聚氨酯、硅溶胶、光引发剂和去离子水混合均匀后加入消泡剂和分散剂,搅拌均匀,制得水性面漆;
第四步、在TPO一侧表面涂覆水性底漆,在紫外光1kW,800mJ/cm2下照射30s,形成水性面漆层,之后涂覆水性面漆,在紫外光照下照射30s,固化后形成水性面漆层,烘干,之后在TPO另一侧表面复合聚烯烃海绵,制得低VOC的TPO汽车内饰材料。
对比例1
本对比例与实施例4相比,采用溶剂型聚氨酯漆进行涂覆。
对比例2
对实施例4-6和对比例1制备出的内饰材料按照TS-BD-003(车内零部件挥发性有机化合物的测试方法-袋子法)规定的方法,测定内饰材料的VOC含量和疏水性能,所得结果如表1所示;
表1
从上表1中能够看出实施例4-6制备出汽车内饰材料散发的VOC较低,符合环保要求,而且具有优异的疏水性能。
以上内容仅仅是对本发明的构思所作的举例和说明,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,只要不偏离发明的构思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 (5)
1.一种低VOC的TPO汽车内饰材料,从下往上依次为聚烯烃海绵层、TPO表层和水漆层,所述水汽层包括水性底漆层和水性面漆层,其特征在于:所述水性底漆层包括如下重量份原料:75-100份改性聚氨酯,0.1-0.8份消泡剂,0.3-0.5份分散剂,5-10份纳米碳酸钙,2-5份硅溶胶,1.2-2.0份光引发剂(2959),30-50份去离子水;
所述水性面漆层包括如下重量份原料:75-100份改性聚氨酯,0.1-0.8份消泡剂,0.3-0.5份分散剂,2-5份硅溶胶,1.2-2.0份光引发剂(2959),30-50份去离子水;
所述改性聚氨酯包括如下步骤制成:
将聚丙二醇、1,4-丁二醇、二羟甲基丙酸和二元醇加入三口烧瓶中,通入氮气,升温至80℃以200r/min的转速磁力搅拌2h,加入异佛尔酮二异氰酸酯和二月桂酸二丁基锡,保温反应3h,反应结束后加入丙酮和三乙胺,搅拌30min,之后以1000r/min的转速匀速搅拌并加入去离子水和乙二胺,搅拌1h,制得乳液,在温度50℃下、真空度0.09MPa下除去丙酮,制得改性聚氨酯。
2.根据权利要求1所述的一种低VOC的TPO汽车内饰材料,其特征在于,所述聚丙二醇、1,4-丁二醇、二羟甲基丙酸、异佛尔酮二异氰酸酯、三乙胺、乙二胺和二元醇的用量比为20g∶4.10-4.12g∶2.02-2.06g∶22.23g∶1.57-1.60g∶1g∶4.24-4.32g,二月桂酸二丁基锡的用量为单体重量和的3-5%。
3.根据权利要求1所述的一种低VOC的TPO汽车内饰材料,其特征在于,所述二元醇包括如下步骤制成:
步骤S1、将六氟正丁醇加入装有丙酮的三口烧瓶中,通入氮气,升温至80℃,在200r/min的转速下匀速搅拌并加入L-赖氨酸三异氰酸酯和二月桂酸二丁基锡,匀速搅拌并保温反应3h,反应结束后降温至室温,加入二乙醇胺,继续搅拌并反应20min,旋蒸除去溶剂,制得中间体1;
步骤S2、将衣康酸和丙烯酸羟乙酯加入装有甲苯的四口烧瓶中,升温至60℃,氮气气氛下加入对甲苯磺酸,匀速搅拌并反应4h,反应结束后升温至70℃,继续搅拌并反应30min,反应结束后用无水硫酸镁除去水,蒸出溶剂,在40℃下抽真空4h,制得中间体2;
步骤S3、将中间体2加入三口烧瓶中,之后加入二氯亚砜,回流反应12h,反应结束后旋蒸除去剩余二氯亚砜,制得滤饼,之后加入四氢呋喃中,过滤,旋蒸除去溶剂,制得中间体3;
步骤S4、将中间体3加入四氢呋喃中,冰水浴下缓慢滴加至浓氨水中,室温下匀速搅拌24h,反应结束后减压蒸出四氢呋喃,用二氯甲烷萃取三次,有机层洗涤后干燥、重结晶,之后将制得的化合物采用霍夫曼降解反应制成中间体4;
步骤S5、将中间体4和中间体1加入四氢呋喃中,室温下匀速搅拌并反应30-45min,旋蒸除去溶剂,制得中间体5,控制中间体4和中间体1的摩尔比为1∶1。
4.根据权利要求1所述的一种低VOC的TPO汽车内饰材料,其特征在于:步骤S1中控制六氟正丁醇、L-赖氨酸三异氰酸酯和二乙醇胺的摩尔比为1∶1∶1,二月桂酸二丁基锡的用量为六氟正丁醇重量的1-2%,步骤S2中控制衣康酸、丙烯酸羟乙酯、对甲苯磺酸和甲苯的用量比为0.1mol∶0.1mol∶0.02g∶20mL,步骤S3中控制中间体2和二氯亚砜的摩尔比为0.1-0.2mol∶0.4-0.5mol,步骤S4中控制中间体3、浓氨水和四氢呋喃的用量比为0.1mol∶200mL∶50mL。
5.根据权利要求1所述的一种低VOC的TPO汽车内饰材料的生产工艺,其特征在于:包括如下步骤:
第一步、按重量份计,将20-50份半交联TPO、10-30份聚丙烯、10-30份聚乙烯、1-3份光稳定剂(UV-119)、10-20份纳米碳酸钙、10-15份硬脂酸类助剂和5-10份色母粒混合均匀后加入挤出机中,挤出后形成TPO薄膜,电晕处理后制得TPO表层;
第二步、将改性聚氨酯、纳米碳酸钙、硅溶胶、光引发剂和去离子水混合均匀后加入消泡剂和分散剂,搅拌均匀,制得水性底漆;
第三步、将改性聚氨酯、硅溶胶、光引发剂和去离子水混合均匀后加入消泡剂和分散剂,搅拌均匀,制得水性面漆;
第四步、在TPO一侧表面涂覆水性底漆,在紫外光(1kW,800mJ/cm2)照下照射30s,形成水性底漆层,之后涂覆水性面漆,在紫外光照下照射30s,固化后形成水性面漆层,烘干,之后在TPO另一侧表面复合聚烯烃海绵,制得低VOC的TPO汽车内饰材料。
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