CN114536887A - 一种覆膜铁及其加工工艺 - Google Patents
一种覆膜铁及其加工工艺 Download PDFInfo
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- CN114536887A CN114536887A CN202210119770.2A CN202210119770A CN114536887A CN 114536887 A CN114536887 A CN 114536887A CN 202210119770 A CN202210119770 A CN 202210119770A CN 114536887 A CN114536887 A CN 114536887A
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 138
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 69
- 238000005516 engineering process Methods 0.000 title claims abstract description 26
- 238000012545 processing Methods 0.000 title claims abstract description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 147
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 64
- 229920000139 polyethylene terephthalate Polymers 0.000 claims abstract description 61
- 229920002799 BoPET Polymers 0.000 claims abstract description 39
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 34
- 238000002791 soaking Methods 0.000 claims abstract description 23
- 238000003851 corona treatment Methods 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 238000009998 heat setting Methods 0.000 claims abstract description 11
- 238000005266 casting Methods 0.000 claims abstract description 9
- 238000013329 compounding Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000004593 Epoxy Substances 0.000 claims abstract description 4
- 238000001125 extrusion Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 134
- 239000000243 solution Substances 0.000 claims description 79
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 66
- 238000001035 drying Methods 0.000 claims description 47
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 46
- 235000019441 ethanol Nutrition 0.000 claims description 37
- ZRALSGWEFCBTJO-UHFFFAOYSA-N Guanidine Chemical compound NC(N)=N ZRALSGWEFCBTJO-UHFFFAOYSA-N 0.000 claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 24
- 229910052757 nitrogen Inorganic materials 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 23
- -1 3-triethoxysilylpropylamino Chemical group 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 16
- 238000004140 cleaning Methods 0.000 claims description 16
- 239000002243 precursor Substances 0.000 claims description 16
- 238000000861 blow drying Methods 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 14
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 claims description 13
- 229960000789 guanidine hydrochloride Drugs 0.000 claims description 12
- PJJJBBJSCAKJQF-UHFFFAOYSA-N guanidinium chloride Chemical compound [Cl-].NC(N)=[NH2+] PJJJBBJSCAKJQF-UHFFFAOYSA-N 0.000 claims description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 11
- CHJJGSNFBQVOTG-UHFFFAOYSA-N N-methyl-guanidine Natural products CNC(N)=N CHJJGSNFBQVOTG-UHFFFAOYSA-N 0.000 claims description 10
- SWSQBOPZIKWTGO-UHFFFAOYSA-N dimethylaminoamidine Natural products CN(C)C(N)=N SWSQBOPZIKWTGO-UHFFFAOYSA-N 0.000 claims description 10
- 229960004198 guanidine Drugs 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 238000004821 distillation Methods 0.000 claims description 9
- 230000001678 irradiating effect Effects 0.000 claims description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 8
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 6
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- 150000003242 quaternary ammonium salts Chemical class 0.000 abstract description 3
- 125000003700 epoxy group Chemical group 0.000 abstract description 2
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- 125000002795 guanidino group Chemical group C(N)(=N)N* 0.000 abstract 1
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 238000000967 suction filtration Methods 0.000 description 11
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- 230000000052 comparative effect Effects 0.000 description 9
- 150000002505 iron Chemical class 0.000 description 8
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- 229910052751 metal Inorganic materials 0.000 description 5
- 238000002390 rotary evaporation Methods 0.000 description 5
- 125000001309 chloro group Chemical group Cl* 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000003365 glass fiber Substances 0.000 description 4
- 150000003512 tertiary amines Chemical class 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 125000002947 alkylene group Chemical group 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
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- 150000001875 compounds Chemical class 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000004594 Masterbatch (MB) Substances 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
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- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
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- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000015784 hyperosmotic salinity response Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- YWFWDNVOPHGWMX-UHFFFAOYSA-N n,n-dimethyldodecan-1-amine Chemical compound CCCCCCCCCCCCN(C)C YWFWDNVOPHGWMX-UHFFFAOYSA-N 0.000 description 1
- 238000010534 nucleophilic substitution reaction Methods 0.000 description 1
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- 239000012266 salt solution Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 210000002489 tectorial membrane Anatomy 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
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Abstract
本发明公开了一种覆膜铁及其加工工艺;本申请制备的覆膜铁具有高粘结性、优异的抗菌性和热稳定性,制备工艺不挥发有机溶剂,安全环保。包括以下步骤:S1:对PET进行表面刻蚀;S2:取步骤S1处理过的PET浸泡于改性溶液中,进行表面接枝反应;S3在二氧化硅表面引入环氧基和季铵盐,形成环氧化二氧化硅;S4:在环氧化二氧化硅表面继续引入胍基,形成胍基化二氧化硅;S5:将改性PET、胍基化二氧化硅混合均匀,于双螺杆挤出机中进行挤出铸片,先进行纵向拉伸,再进行横向拉伸膜,最后热定型,对膜表面进行电晕处理后,即为PET薄膜;S6:将PET薄膜与铁板进行热复合后,即为覆膜铁。
Description
技术领域
本发明涉及覆膜铁技术领域,具体为一种覆膜铁及其加工工艺。
背景技术
在制罐行业,通常会在金属表面涂覆有色涂料达到美化的现象,在内表面涂覆热固性涂料,形成涂膜层,虽然可以防止内容物的腐蚀,但是形成涂膜层需要挥发掉有机溶剂,必然会影响环境。
而覆膜铁是利用高温高压将金属板和塑料薄膜贴合在一起的加工技术,可以避免传统工艺的套色、烘烤工艺,常常应用于食品包装、汽车、家居建材等领域,可以增强包装物的稳定性以及美化性。
覆膜铁通常又可分为黏合覆膜铁以及熔融覆膜铁,黏合覆膜铁在制备过程中需要加入粘合剂,和熔融覆膜铁直接利用铁板与薄膜进行复合,所以熔融覆膜铁的使用频率较高。
而覆膜铁最常用薄膜为聚丙烯(PP)和聚对苯二甲酸乙二醇酯(PET),两者可以经受高摩擦和高温的作用,同时具有较强的阻隔性,可以很好的保持内容物的风味,同时在高温杀菌工艺下,薄膜不会脱落、变色等。
而PET薄膜在制备过程中,需要经过纵向拉伸和横向拉伸,这会导致PET薄膜的结晶表面活性低、表面光滑、熔点高,使PET薄膜难以与金属板进行热复合,因此需要提高PET与金属板之间的粘合性,因此提高PET薄膜的表面活性,以增强PET薄膜与金属材料之间的粘结是亟待解决的问题。
发明内容
本发明的目的在于提供一种覆膜铁及其加工工艺,以解决上述背景技术中提出的问题。
为了解决上述技术问题,本发明提供如下技术方案:
一种覆膜铁及其加工工艺,包括以下步骤:
S1:将碳酸钠和氢氧化钠溶于去离子水中,升温至70-90℃,将PET浸泡在溶液中1-1.5h,用去离子水和乙醇洗涤,吹干、备用;
S2:取步骤S1处理过的PET浸泡于6-(3-三乙氧基甲硅烷基丙基氨基)-1,3,5-三嗪-2,4-双叠氮的乙醇溶液中30s,吹干,在紫外灯下照射130-180s后,清洗、吹干后,置于6-(3-三乙氧基甲硅烷基丙基氨基)-1,3,5-三嗪-2,4-二硫醇钠的水溶液中反应10-15min,清洗、吹干,即为改性PET;
S3:将二氧化硅溶于甲苯溶液中,通入氮气,加入KH-550,在80-100℃反应4-6h,抽滤、60℃干燥2h后,即为氨基化二氧化硅;继续通入氮气,将氨基化二氧化硅溶于无水乙醇中,缓慢加入环氧氯丙烷,反应10-14h后,在30-50℃进行减压蒸馏,用丙酮洗涤后,溶于无水甲醇中,升温至50-60℃,缓慢加入环氧氯丙烷的乙醇溶液,继续反应6-9h,降温、旋蒸、无水乙醚洗脱、干燥24h,即为环氧化二氧化硅;
S4:将环氧化二氧化硅溶于无水甲苯溶液中,超声分散0.5-1h,加入胍基前驱体,通入氮气,升温至100-120℃,反应10-14h,冷却、离心、甲苯洗涤、80℃干燥24h,即为胍基化二氧化硅;
S5:将改性PET、胍基化二氧化硅混合均匀,于双螺杆挤出机中进行挤出铸片,先进行纵向拉伸,再进行横向拉伸膜,最后热定型,对膜表面进行电晕处理后,即为PET薄膜;
S6:将PET薄膜与铁板进行热复合后,即为覆膜铁。
步骤S1、S2中的PET是指PET母料。
进一步优化的方案,步骤S4中,胍基前驱体的加工工艺为:将盐酸胍溶于无水乙醇溶液中,缓慢加入乙醇钠溶液,抽滤、除去乙醇溶剂。
进一步优化的方案,所述覆膜铁所需材料包括,以重量计:PET50-80份、胍基化二氧化硅20-50份。
进一步优化的方案,步骤S3中,环氧氯丙烷和氨基化二氧化硅的质量比为3:1;步骤S4中,胍基前驱体和环氧化二氧化硅的质量比为2:1。
进一步优化的方案,所述铁板为马口铁、冷轧铁板中的一种或多种。
进一步优化的方案,所述PET薄膜厚度为20-25μm。
进一步优化的方案:步骤S5中,电晕处理参数为:输出电功率为5.7kw;输出电压为8.2kw;处理时间为3-10s。
进一步优化的方案,步骤S5中,纵向拉伸温度为70-80℃,拉伸比为3-4,横向拉伸温度为90-100℃,拉伸比为2-3,热定型温度为230-250℃;步骤S6中,热复合温度为230-260℃。
进一步优化的方案,根据以上任意一项所述的一种覆膜铁的加工工艺制备的覆膜铁。
本申请利用PET薄膜与铁板复合制备出覆膜铁,但是PET本身具有熔点较高而表面活性低的性能,导致PET与铁板难以复合,所以本申请首先对PET进行化学刻蚀处理,使PET表面产生孔洞,这些孔洞亲附金属铁板,增强了铁板与PET薄膜之间的附着力。随后在PET表面接枝了TTD和TTA,利用N-H键进行紫外光接枝TTA,随后利用TTA和TTD之间的脱水缩合反应,从而将TTD继续接枝在PET表面,使PET表面具有-SH基团,吸附金属离子(铁卷)来提高PET薄膜的粘性(吸附性)。
其次,利用硅烷偶联剂KH-550对二氧化硅进行表面改性,引入-NH2基团,提高了二氧化硅的分散性,接着使用环氧氯丙烷与-NH2的之间取代反应,使伯胺转变为叔胺,表面与进入氯原子,再利用环氧氯丙烷取代叔胺,使叔胺变为季铵盐,同时引入了环氧烷,利用二氧化硅表面的环氧烷与PET表面游离的羧基进行反应,提高了PET与二氧化硅之间的交联度,可以提高覆膜铁的抗冲击力和硬度,季铵盐的引入增强了覆膜铁的抗菌性,同时二氧化硅的引入是覆膜铁具有防光反射的作用。
在PET表面接枝其他基团时,会降低PET的热稳定性,因此本申请利用二氧化硅表面引入的氯原子与胍进行亲核取代反应,从而引入胍基,可以提高覆膜铁的热稳定性,因为本申请是在二氧化硅链段的两端引入的氯原子,因此两处的氯原子均能和胍基反应,与胍基发生交联,在链段两端引入结构对称的胍基,从而不会影响胍基本身的电子效应,阻挡了受热过程中羟基对C-N碱的攻击,从而提高了PET薄膜的热稳定性。
最后对PET薄膜表面进行电晕处理,增强PWT薄膜表面的浸润性,可以提高PET薄膜的表面能,从而提高了PET薄膜与铁板之间的粘结力。
与现有技术相比,本发明所达到的有益效果是:本发明制备的覆膜铁具有高粘结性、优异的抗菌性和热稳定性。制备工艺不挥发有机溶剂,安全环保。
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做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1:一种覆膜铁及其加工工艺,包括以下步骤:
S1:配置10%的碳酸钠溶液和10%的氢氧化钠溶液,两种溶液1:1混合均匀后,升温至70℃,将PET浸泡在溶液中1h,用去离子水和乙醇洗涤,吹干、备用;
S2:将0.05份6-(3-三乙氧基甲硅烷基丙基氨基)-1,3,5-三嗪-2,4-双叠氮溶于100份的乙醇溶液中,取步骤S1处理过的PET浸泡于TTA的乙醇溶液中30s,吹干,在辐照强度为2.5J/cm2,波长为356nm下紫外灯照射130s,用乙醇对其进行清洗、吹干;
S3:将0.1份6-(3-三乙氧基甲硅烷基丙基氨基)-1,3,5-三嗪-2,4-二硫醇钠溶于100份去离子水中,将吹干后的PET浸泡于TTD的水溶液中反应10min,清洗、吹干,即为改性PET;
S4:将4份盐酸胍溶于40份无水乙醇溶液中,在20℃进行搅拌,使其溶解,边搅拌边缓慢加入40份1.1mol/L的乙醇钠溶液,抽滤,除去滤液中的乙醇溶剂,即为胍基前驱体;
S5:将二氧化硅在60℃干燥12h后,取1份二氧化硅溶于25份甲苯溶液中,室温反应0.5h后,进行抽真空,通入氮气,加入1份KH-550,在80℃回流反应4h,抽滤、60℃干燥2h后,即为氨基化二氧化硅;继续通入氮气,将8份氨基化二氧化硅溶于40份无水乙醇中,缓慢加入16份环氧氯丙烷,反应10h后,在30℃进行减压蒸馏2h,用丙酮洗涤3次后,溶于10份无水甲醇中,升温至50℃,将8份环氧氯丙烷溶于10份无水乙醇中,加入至上述溶液中,继续反应6h,降温、旋蒸、无水乙醚进行洗脱5次、120℃干燥24h,即为环氧化二氧化硅;
S6:将1份环氧化二氧化硅溶于25份无水甲苯溶液中,超声分散0.5h,加入2份胍基前驱体,通入氮气,升温至100℃,反应10h,冷却、离心、甲苯洗涤、80℃干燥24h,即为胍基化二氧化硅;
S7:将50份改性PET、50份胍基化二氧化硅混合均匀,于双螺杆挤出机中进行挤出铸片,先进行纵向拉伸,拉伸温度为70℃,拉伸比为3,再进行横向拉伸膜,温度为90℃,拉伸比为2,在230℃进行热定型,对膜表面进行电晕处理,电晕处理参数为:输出电功率为5.7kw;输出电压为8.2kw;处理时间为3s,即为PET薄膜;
S8:将PET薄膜与冷轧铁板在230℃进行热复合后,即为覆膜铁。
实施例2:一种覆膜铁及其加工工艺,包括以下步骤:
S1:配置10%的碳酸钠溶液和10%的氢氧化钠溶液,两种溶液1:1混合均匀后,升温至75℃,将PET浸泡在溶液中1-1.5h,用去离子水和乙醇洗涤,吹干、备用;
S2:将0.06份6-(3-三乙氧基甲硅烷基丙基氨基)-1,3,5-三嗪-2,4-双叠氮溶于105份的乙醇溶液中,取步骤S1处理过的PET浸泡于TTA的乙醇溶液中30s,吹干,在辐照强度为2.5J/cm2,波长为356nm下紫外灯照射140s,用乙醇对其进行清洗、吹干;
S3:将0.2份6-(3-三乙氧基甲硅烷基丙基氨基)-1,3,5-三嗪-2,4-二硫醇钠溶于105份去离子水中,将吹干后的PET浸泡于TTD的水溶液中反应11min,清洗、吹干,即为改性PET;
S4:将5份盐酸胍溶于45份无水乙醇溶液中,在21℃进行搅拌,使其溶解,边搅拌边缓慢加入45份1.1mol/L的乙醇钠溶液,抽滤,除去滤液中的乙醇溶剂,即为胍基前驱体;
S5:将二氧化硅在60℃干燥12h后,取2份二氧化硅溶于30份甲苯溶液中,室温反应0.6h后,进行抽真空,通入氮气,加入1.5份KH-550,在85℃回流反应4.5h,抽滤、60℃干燥2h后,即为氨基化二氧化硅;继续通入氮气,将9份氨基化二氧化硅溶于45份无水乙醇中,缓慢加入18份环氧氯丙烷,反应11h后,在35℃进行减压蒸馏2.5h,用丙酮洗涤3次后,溶于11份无水甲醇中,升温至51℃,将9份环氧氯丙烷溶于11份无水乙醇中,加入至上述溶液中,继续反应6.5h,降温、旋蒸、无水乙醚进行洗脱5次、120℃干燥24h,即为环氧化二氧化硅;
S6:将2份环氧化二氧化硅溶于30份无水甲苯溶液中,超声分散0.6h,加入4份胍基前驱体,通入氮气,升温至105℃,反应11h,冷却、离心、甲苯洗涤、80℃干燥24h,即为胍基化二氧化硅;
S7:将60份改性PET、40份胍基化二氧化硅混合均匀,于双螺杆挤出机中进行挤出铸片,先进行纵向拉伸,拉伸温度为75℃,拉伸比为3.5,再进行横向拉伸膜,温度为95℃,拉伸比为2.5,在235℃进行热定型,对膜表面进行电晕处理,电晕处理参数为:输出电功率为5.7kw;输出电压为8.2kw;处理时间为5s,即为PET薄膜;
S8:将PET薄膜与冷轧铁板在240℃进行热复合后,即为覆膜铁。
实施例3:一种覆膜铁及其加工工艺,包括以下步骤:
S1:配置10%的碳酸钠溶液和10%的氢氧化钠溶液,两种溶液1:1混合均匀后,升温至80℃,将PET浸泡在溶液中1.2h,用去离子水和乙醇洗涤,吹干、备用;
S2:将0.07份6-(3-三乙氧基甲硅烷基丙基氨基)-1,3,5-三嗪-2,4-双叠氮溶于110份的乙醇溶液中,取步骤S1处理过的PET浸泡于TTA的乙醇溶液中30s,吹干,在辐照强度为2.5J/cm2,波长为356nm下紫外灯照射150s,用乙醇对其进行清洗、吹干;
S3:将0.3份6-(3-三乙氧基甲硅烷基丙基氨基)-1,3,5-三嗪-2,4-二硫醇钠溶于110份去离子水中,将吹干后的PET浸泡于TTD的水溶液中反应12min,清洗、吹干,即为改性PET;
S4:将6份盐酸胍溶于50份无水乙醇溶液中,在22℃进行搅拌,使其溶解,边搅拌边缓慢加入50份1.1mol/L的乙醇钠溶液,抽滤,除去滤液中的乙醇溶剂,即为胍基前驱体;
S5:将二氧化硅在60℃干燥12h后,取3份二氧化硅溶于35份甲苯溶液中,室温反应0.7h后,进行抽真空,通入氮气,加入2份KH-550,在90℃回流反应5h,抽滤、60℃干燥2h后,即为氨基化二氧化硅;继续通入氮气,将10份氨基化二氧化硅溶于50份无水乙醇中,缓慢加入20份环氧氯丙烷,反应12h后,在30-50℃进行减压蒸馏3h,用丙酮洗涤3次后,溶于15份无水甲醇中,升温至55℃,将10份环氧氯丙烷溶于15份无水乙醇中,加入至上述溶液中,继续反应8h,降温、旋蒸、无水乙醚进行洗脱5次、120℃干燥24h,即为环氧化二氧化硅;
S6:将5份环氧化二氧化硅溶于35份无水甲苯溶液中,超声分散0.7h,加入10份胍基前驱体,通入氮气,升温至110℃,反应12h,冷却、离心、甲苯洗涤、80℃干燥24h,即为胍基化二氧化硅;
S7:将65份改性PET、35份胍基化二氧化硅混合均匀,于双螺杆挤出机中进行挤出铸片,先进行纵向拉伸,拉伸温度为75℃,拉伸比为3,再进行横向拉伸膜,温度为95℃,拉伸比为2,在2400℃进行热定型,对膜表面进行电晕处理,电晕处理参数为:输出电功率为5.7kw;输出电压为8.2kw;处理时间为6s,即为PET薄膜;
S8:将PET薄膜与冷轧铁板在250℃进行热复合后,即为覆膜铁。
实施例4:一种覆膜铁及其加工工艺,包括以下步骤:
S1:配置10%的碳酸钠溶液和10%的氢氧化钠溶液,两种溶液1:1混合均匀后,升温至70-90℃,将PET浸泡在溶液中1-1.5h,用去离子水和乙醇洗涤,吹干、备用;
S2:将0.08份6-(3-三乙氧基甲硅烷基丙基氨基)-1,3,5-三嗪-2,4-双叠氮溶于115份的乙醇溶液中,取步骤S1处理过的PET浸泡于TTA的乙醇溶液中30s,吹干,在辐照强度为2.5J/cm2,波长为356nm下紫外灯照射175s,用乙醇对其进行清洗、吹干;
S3:将0.7份6-(3-三乙氧基甲硅烷基丙基氨基)-1,3,5-三嗪-2,4-二硫醇钠溶于115份去离子水中,将吹干后的PET浸泡于TTD的水溶液中反应14min,清洗、吹干,即为改性PET;
S4:将6份盐酸胍溶于58份无水乙醇溶液中,在24℃进行搅拌,使其溶解,边搅拌边缓慢加入58份1.1mol/L的乙醇钠溶液,抽滤,除去滤液中的乙醇溶剂,即为胍基前驱体;
S5:将二氧化硅在60℃干燥12h后,取5份二氧化硅溶于43份甲苯溶液中,室温反应0.7h后,进行抽真空,通入氮气,加入2.5份KH-550,在95℃回流反应5.8h,抽滤、60℃干燥2h后,即为氨基化二氧化硅;继续通入氮气,将12份氨基化二氧化硅溶于55份无水乙醇中,缓慢加入24份环氧氯丙烷,反应13h后,在45℃进行减压蒸馏3.8h,用丙酮洗涤3次后,溶于18份无水甲醇中,升温至58℃,将12份环氧氯丙烷溶于18份无水乙醇中,加入至上述溶液中,继续反应8.5h,降温、旋蒸、无水乙醚进行洗脱5次、120℃干燥24h,即为环氧化二氧化硅;
S6:将7份环氧化二氧化硅溶于38份无水甲苯溶液中,超声分散0.8h,加入14份胍基前驱体,通入氮气,升温至115℃,反应13.5h,冷却、离心、甲苯洗涤、80℃干燥24h,即为胍基化二氧化硅;
S7:将70份改性PET、30份胍基化二氧化硅混合均匀,于双螺杆挤出机中进行挤出铸片,先进行纵向拉伸,拉伸温度为75℃,拉伸比为4,再进行横向拉伸膜,温度为95℃,拉伸比为3,在245℃进行热定型,对膜表面进行电晕处理,电晕处理参数为:输出电功率为5.7kw;输出电压为8.2kw;处理时间为8s,即为PET薄膜;
S8:将PET薄膜与冷轧铁板在255℃进行热复合后,即为覆膜铁。
实施例5:一种覆膜铁及其加工工艺,包括以下步骤:
S1:配置10%的碳酸钠溶液和10%的氢氧化钠溶液,两种溶液1:1混合均匀后,升温至90℃,将PET浸泡在溶液中1.5h,用去离子水和乙醇洗涤,吹干、备用;
S2:将1份6-(3-三乙氧基甲硅烷基丙基氨基)-1,3,5-三嗪-2,4-双叠氮溶于120份的乙醇溶液中,取步骤S1处理过的PET浸泡于TTA的乙醇溶液中30s,吹干,在辐照强度为2.5J/cm2,波长为356nm下紫外灯照射180s,用乙醇对其进行清洗、吹干;
S3:将0.8份6-(3-三乙氧基甲硅烷基丙基氨基)-1,3,5-三嗪-2,4-二硫醇钠溶于120份去离子水中,将吹干后的PET浸泡于TTD的水溶液中反应15min,清洗、吹干,即为改性PET;
S4:将10份盐酸胍溶于60份无水乙醇溶液中,在25℃进行搅拌,使其溶解,边搅拌边缓慢加入60份1.1mol/L的乙醇钠溶液,抽滤,除去滤液中的乙醇溶剂,即为胍基前驱体;
S5:将二氧化硅在60℃干燥12h后,取6份二氧化硅溶于45份甲苯溶液中,室温反应1h后,进行抽真空,通入氮气,加入3份KH-550,在100℃回流反应6h,抽滤、60℃干燥2h后,即为氨基化二氧化硅;继续通入氮气,将15份氨基化二氧化硅溶于60份无水乙醇中,缓慢加入30份环氧氯丙烷,反应14h后,在50℃进行减压蒸馏4h,用丙酮洗涤3次后,溶于20份无水甲醇中,升温至60℃,将15份环氧氯丙烷溶于20份无水乙醇中,加入至上述溶液中,继续反应9h,降温、旋蒸、无水乙醚进行洗脱5次、120℃干燥24h,即为环氧化二氧化硅;
S6:将8份环氧化二氧化硅溶于40份无水甲苯溶液中,超声分散1h,加入16份胍基前驱体,通入氮气,升温至120℃,反应14h,冷却、离心、甲苯洗涤、80℃干燥24h,即为胍基化二氧化硅;
S7:将80份改性PET、20份胍基化二氧化硅混合均匀,于双螺杆挤出机中进行挤出铸片,先进行纵向拉伸,拉伸温度为80℃,拉伸比为4,再进行横向拉伸膜,温度为100℃,拉伸比为3,在250℃进行热定型,对膜表面进行电晕处理,电晕处理参数为:输出电功率为5.7kw;输出电压为8.2kw;处理时间为3-10s,即为PET薄膜;
S8:将PET薄膜与冷轧铁板260℃进行热复合后,即为覆膜铁。
对比例
对比例1:一种覆膜铁及其加工工艺,包括以下步骤:
S1:配置10%的碳酸钠溶液和10%的氢氧化钠溶液,两种溶液1:1混合均匀后,升温至70℃,将PET浸泡在溶液中1h,用去离子水和乙醇洗涤,吹干、备用;
S2:将0.05份6-(3-三乙氧基甲硅烷基丙基氨基)-1,3,5-三嗪-2,4-双叠氮溶于100份的乙醇溶液中,取步骤S1处理过的PET浸泡于TTA的乙醇溶液中30s,吹干,在辐照强度为2.5J/cm2,波长为356nm下紫外灯照射130s,用乙醇对其进行清洗、吹干;
S3:将0.1份6-(3-三乙氧基甲硅烷基丙基氨基)-1,3,5-三嗪-2,4-二硫醇钠溶于100份去离子水中,将吹干后的PET浸泡于TTD的水溶液中反应10min,清洗、吹干,即为改性PET;
S4:将二氧化硅在60℃干燥12h后,取1份二氧化硅溶于25份甲苯溶液中,室温反应0.5h后,进行抽真空,通入氮气,加入1份KH-550,在80℃回流反应4h,抽滤、60℃干燥2h后,即为氨基化二氧化硅;继续通入氮气,将8份氨基化二氧化硅溶于40份无水乙醇中,缓慢加入16份环氧氯丙烷,反应10h后,在30℃进行减压蒸馏2h,用丙酮洗涤3次后,缓慢加入16份十二烷基二甲胺,升温至80℃,回流反应10h后,在60℃进行减压蒸馏2h,用丙酮重结晶,40℃干燥6h,即为季铵化二氧化硅;
S5:将50份改性PET、50份季铵化二氧化硅混合均匀,于双螺杆挤出机中进行挤出铸片,先进行纵向拉伸,拉伸温度为70℃,拉伸比为3,再进行横向拉伸膜,温度为90℃,拉伸比为2,在230℃进行热定型,对膜表面进行电晕处理,电晕处理参数为:输出电功率为5.7kw;输出电压为8.2kw;处理时间为3s,即为PET薄膜;
S6:将PET薄膜与冷轧铁板在230℃进行热复合后,即为覆膜铁。
对比例2:不加入环氧化二氧化硅,也不对PET薄膜进行处理,直接将PET薄膜与冷轧铁板在230℃进行热复合。
实验数据
耐水:将样品在125℃,去离子水中蒸煮1h,观察PET薄膜脱落情况。
耐酸:将样品在125℃,3%的乙酸溶液中蒸煮1h,观察PET薄膜脱落情况。
耐盐:将样品在125℃,3%的盐水溶液中蒸煮1h,观察PET薄膜脱落情况。
表1实施例1-5、对比例1、对比例2各项检测结果
结论:
1.实施例1-5与对比例1对比,对比例1直接将二氧化硅表面的-NH2直接进行季铵化,没有引入环氧基,所以二氧化硅和PET不会发生交联,导致覆膜铁机械性能小幅度下降。
2.实施例1-5与对比例2对比,对比例2没有对PET进行接枝改性,也没有加入胍基化二氧化硅,导致覆膜铁在水溶液、酸溶液、盐溶液中膜层脱落,降低了PET薄膜和冷轧铁板之间的粘结力,同时缺少了胍基化二氧化硅,导致覆膜铁的机械强度也大幅度下降。
最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (9)
1.一种覆膜铁的加工工艺,其特征在于:包括以下步骤:
S1:将碳酸钠和氢氧化钠溶于去离子水中,升温至70-90℃,将PET浸泡在溶液中1-1.5h,用去离子水和乙醇洗涤,吹干、备用;
S2:取步骤S1处理过的PET浸泡于6-(3-三乙氧基甲硅烷基丙基氨基)-1,3,5-三嗪-2,4-双叠氮的乙醇溶液中30s,吹干,在紫外灯下照射130-180s后,清洗、吹干后,置于6-(3-三乙氧基甲硅烷基丙基氨基)-1,3,5-三嗪-2,4-二硫醇钠的水溶液中反应10-15min,清洗、吹干,即为改性PET;
S3:将二氧化硅溶于甲苯溶液中,通入氮气,加入KH-550,在80-100℃反应4-6h,抽滤、60℃干燥2h后,即为氨基化二氧化硅;继续通入氮气,将氨基化二氧化硅溶于无水乙醇中,缓慢加入环氧氯丙烷,反应10-14h后,在30-50℃进行减压蒸馏,用丙酮洗涤后,溶于无水甲醇中,升温至50-60℃,缓慢加入环氧氯丙烷的乙醇溶液,继续反应6-9h,降温、旋蒸、无水乙醚洗脱、干燥24h,即为环氧化二氧化硅;
S4:将环氧化二氧化硅溶于无水甲苯溶液中,超声分散0.5-1h,加入胍基前驱体,通入氮气,升温至100-120℃,反应10-14h,冷却、离心、甲苯洗涤、80℃干燥24h,即为胍基化二氧化硅;
S5:将改性PET、胍基化二氧化硅混合均匀,于双螺杆挤出机中进行挤出铸片,先进行纵向拉伸,再进行横向拉伸膜,最后热定型,对膜表面进行电晕处理后,即为PET薄膜;
S6:将PET薄膜与铁板进行热复合后,即为覆膜铁。
2.根据权利要求1所述的一种覆膜铁的加工工艺,其特征在于:步骤S4中,胍基前驱体的加工工艺为:将盐酸胍溶于无水乙醇溶液中,缓慢加入乙醇钠溶液,抽滤、除去乙醇溶剂。
3.根据权利要求1所述的一种覆膜铁的加工工艺,其特征在于:所述覆膜铁所需材料包括,以重量计:PET50-80份、胍基化二氧化硅20-50份。
4.根据权利要求1所述的一种覆膜铁的加工工艺,其特征在于:步骤S3中,环氧氯丙烷和氨基化二氧化硅的质量比为3:1;步骤S4中,胍基前驱体和环氧化二氧化硅的质量比为2:1。
5.根据权利要求1所述的一种覆膜铁的加工工艺,其特征在于:所述铁板为马口铁、冷轧铁板中的一种或多种。
6.根据权利要求1所述的一种覆膜铁的加工工艺,其特征在于:所述PET薄膜厚度为20-25μm。
7.根据权利要求1所述的一种覆膜铁的加工工艺,其特征在于:步骤S5中,电晕处理参数为:输出电功率为5.7kw;输出电压为8.2kw;处理时间为3-10s。
8.根据权利要求1所述的一种覆膜铁的加工工艺,其特征在于:步骤S5中,纵向拉伸温度为70-80℃,拉伸比为3-4,横向拉伸温度为90-100℃,拉伸比为2-3,热定型温度为230-250℃;步骤S6中,热复合温度为230-260℃。
9.根据权利要求1-8任意一项所述的一种覆膜铁的加工工艺制备的覆膜铁。
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