CN107903556B - 一种pmma超薄超透薄膜及其制作方法 - Google Patents
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Abstract
本发明涉及PMMA材料应用领域,提供一种PMMA超薄超透薄膜及其制作方法,解决了聚甲基丙烯酸甲酯原料(PMMA)在加工过程成膜过程中对设备要求高、流动性不足、易脆裂的问题。可利用国产挤出压延设备和工艺,替代进口挤出压延设备,利用以下原料组成改性:聚甲基丙烯酸甲酯原料90%、甲基丙烯酸甲酯‑丁二烯‑甲基丙烯酸脂共聚物5%‑8%、聚乙烯接枝马来酸酐PE‑g‑MAH2%‑5%,生产出达到《GBT 18833‑2012道路交通反光膜》中检测方法及标准、厚度为0.05mm‑0.08mm的超薄超透薄膜。
Description
技术领域
本发明涉及PMMA材料应用领域,尤其涉及一种用PMMA制作的超薄超透薄膜及其制作方法。
背景技术
PMMA(聚甲基丙烯酸甲酯,简称PMMA,英文Acrylic,又称做亚克力或有机玻璃)具有机械强度较高、透明度优良,有突出的耐老化性能和良好的化学稳定性等优点,但由于其加工流动性差、硬度高、抗冲击能力弱等性质,使其在加工过程中对设备要求高、流动性不足、易脆裂等原因严重限制了使用范围。
鉴于PMMA原料流动性不足及后续加工难度大、设备投资门槛高等综合因素,国内现有PMMA薄膜,大多数均为注塑和流延加工方法生产,且厚度均在0.5mm以上,达不到高品质交通反光膜的需要。
传统挤出压延工艺,如想实现厚度为0.05mm~0.08mm超薄产品的生产,一般有三种工艺:第一,采用双面柔性光学镜面辊轮对压系统,此类工艺技术,主要掌握在日本企业,且造价高昂;第二,采用一面镜面、一面硅胶辊双辊对压,此工艺所生产的产品应力小,但表面粗糙,表面外观为一面镜面,一面雾面,无法做到超透的镜面效果;第三,采用单镜面辊静电吸附工艺,此工艺生产产品,表面无法完全抛光,存在晶点、流痕等外观缺陷。
常用的塑料增韧方式主要有弹性体增韧、热塑性树脂贯穿网络增韧、无机刚性粒子增韧等方式,其中弹性体增韧采用的橡胶颗粒会带来耐老化缺陷,热塑性树脂贯穿网络增韧效果稳定,主要考虑增韧剂本身特性以及在基体材料中的分散性,无机刚性粒子增韧考虑无机粒子比表面积及无机粒子与树脂之间的结合界面是否良好。
专利文件CN 201010224506.2公开了一种用MBS(甲基丙烯酸甲酯-丁二烯-苯乙烯三元共聚物)做增韧剂改性PMMA材料的方法,但该公开文件中增韧剂MBS添加量在20-30%之间,添加量大,生产费用高,且MBS含有不饱和结构的丁二烯、易受氧气和紫外线的作用而老化,故耐候性差,不宜过多使用,所述改性PMMA材料不适合制作高品质交通反光膜需要。
由于原料改性难度系数及后续加工难度大、设备投资门槛高且行业使用范围窄等综合因素,现有市场超透超薄PMMA薄膜,绝大多数均来自于日本三菱丽阳、日本钟化学、德国赢德固赛等国外PMMA原料厂家直接供应。
隋着国内反光行业的逐渐成熟,加上3M交通标志数码打印技术的推广,作为反光基膜和打印面膜配套产品的PMMA超薄超透薄膜及其延伸的反光电刻膜,会迎来一个全新的增长爆发阶段。但由于原料改性难度系数及后续加工难度大、设备投资门槛高且行业使用范围窄等综合因素,现有市场超透超薄PMMA薄膜,绝大多数均来自于日本三菱丽阳、日本钟化学、德国赢德固赛等国外PMMA原料厂家直接供应。除原料瓶颈外,PMMA超薄超透薄膜所需动辄2000万以上的设备投入,也是造成国内目前无法实现产业化普及的重要原因。本发明,在通过对原料改性后,采用新的压延工艺,即可有效降低设备投入门槛,又能对产品实现镜面抛光,使产品表观达到透明光学效果,满足行业质量需求。
发明内容
因此,针对上述的问题,本发明提供一种PMMA超薄超透薄膜及其制作方法,解决了PMMA在加工过程成膜过程中对设备要求高、流动性不足、易脆裂的问题。
为实现上述目的,本发明采用了以下技术方案:
一种PMMA超薄超透薄膜,由以下重量份的各原料组成:聚甲基丙烯酸甲酯85~95份、增韧剂5~8份、相容剂2~5份。
进一步的改进是:所述增韧剂为甲基丙烯酸甲酯-丁二烯-甲基丙烯酸脂共聚物。
进一步的改进是:所述相容剂为聚乙烯接枝马来酸酐。
进一步的改进是:所述聚甲基丙烯酸甲酯选自三菱、住友或奇美普通级聚甲基丙烯酸甲酯。
一种PMMA超薄超透薄膜的制作方法,包括以下步骤:
(1)原料混合:将聚甲基丙烯酸甲酯85~95份、增韧剂5~8份、相容剂2~5份投入高速混合机内高速搅拌10min~15min,搅拌温度控制在60℃~70℃,得到混合物,经冷混机将混合物温度降至40℃~50℃;
(2)造粒:将步骤(1)制得的混合物经同向平行双螺杆造粒机改性造粒,得到原料粒子,所述同向平行双螺杆的直径20~25mm,螺杆长径比32:1~52:1,造粒温度180℃~200℃;
(3)挤出压延:将步骤(2)制得的原料粒子干燥后由挤出压延设备压延成型,制作出厚度为0.05mm~0.08mm的热熔胶薄膜,所述原料粒子干燥温度控制在80℃~100℃,干燥时长控制在4h~6h;挤出单螺杆温度控制在220℃~240℃,输送段温度控制在230℃~250℃,挤出压力5MPa~12MPa,生产速度为5m/min~30m/min;
(4)成品收卷;
步骤(3)中所述挤出压延设备包括依次排列的单螺杆挤出机(1)、压延设备(2)、成品收卷装置(3),所述压延设备(2)包括依次排列的耐高温塑料薄膜覆膜设备(4)、硅胶辊(5)、镜面辊(6)、镜面辊(7)、冷却辊组(8),硅胶辊(5)和镜面辊(6)之间缝隙正上方设有挤出机模头(9)。
进一步的改进是:所述耐高温塑料薄膜覆膜设备(4)上设有薄膜张力调节装置(10),本发明的PMMA超透超薄薄膜,主要应用于《GBT 18833-2012道路交通反光膜》中的第四、第五和第七类薄膜。
通过采用前述技术方案,本发明的有益效果是:
1、本发明所用材料均为市场普通材料,可通过商业方式获得。本发明将普通PMMA原料经改性后克服了PMMA在加工过程中对设备要求高、流动性不足、易脆裂等的缺点,保留了机械强度较高、透明度优良,有突出的耐老化性能和良好的化学稳定性等优点。
2、所述相容剂优选聚乙烯接枝马来酸酐PE-g-MAH,与甲基丙烯酸甲酯-丁二烯-甲基丙烯酸脂共聚物和PMMA都有优秀的相容性,可以使在PMMA中形成稳均匀的贯穿网络,进一步提高混合材料的相容性和机械强度。
3、所述增韧剂为甲基丙烯酸甲酯-丁二烯-甲基丙烯酸脂共聚物,原料来源广泛。
4、本发明创造性的在现有双辊压延机的基础上增加一套耐高温塑料薄膜设备即可实现PMMA超薄超透薄膜的双镜面压延,设备投入成本降低,且所生产产品既可保证其优异的光学性能和表观质量,又可使其应力降至理想状态,克服了一般PMMA流延膜厚度精度一般,平整性差、横向均匀性一般的缺点。
5、所述PMMA超薄超透薄膜生产方法,材料成本低,设备投入低,经济效益突出。
6、所述PMMA超薄超透薄膜,因其透光率高、雾度低等优异的光学性能,突出的耐候性能,表面硬度高,可提供卓越的耐划伤性、印刷性及剪贴等加工性能,能广泛应用于交通标识、标示板、安全标识、车辆(车牌号、车牌)等领域的反光膜中作为基膜,显著提高反光膜的品质。
附图说明
图1是本发明实施例1中挤出压延设备的结构示意图;
图2是本发明实施例1中的生产流程图。
具体实施方式
以下将结合具体实施例来详细说明本发明的实施方式,借此对本发明如何应用技术手段来解决技术问题,并达成技术效果的实现过程能充分理解并据以实施。
若未特别指明,实施例中所采用的技术手段为本领域技术人员所熟知的常规手段,所采用的试剂和产品均为可商业获得的。
实施例1
1、一种PMMA超薄超透薄膜,由90KG PMMA、15KG甲基丙烯酸甲酯-丁二烯-甲基丙烯酸脂共聚物、5KG聚乙烯接枝马来酸酐PE-g-MAH原料组分组成。
其制备方法为:参考图1及图2,将上述各原料组分投入高速混合机内高速搅拌10min,温度为60℃得到混合物,经冷混机将混合物降至45℃;将混合物加入造粒机的搅拌室中,造粒机采用同向平行双螺杆,螺杆直径20mm,螺杆长径比52:1,造粒温度200℃,通过造粒机制成颗粒;将所述颗粒经充分干燥后通过单螺杆挤出机1熔融挤出,由挤出机模头9进入压延装置2压延,耐高温塑料薄膜覆膜设备4设有薄膜张力调节装置10,用于向硅胶辊5提供耐高温塑料薄膜进行贴合形成镜面,PMMA超薄超透薄膜经挤出机模头9挤出,进入胶辊5与镜面辊6之间进行镜面抛光,然后进入镜面辊6与镜面辊7之间进一步镜面抛光成型,经冷却辊组8冷却导出,进入成品收卷装置3收卷,制作出厚度为0.08mm的超薄、超透薄膜。原料粒子干燥温度120℃,干燥时长4h,;挤出机螺杆温度240℃,输送段温度250℃,挤出压力12MPa;压延生产速度5m/min。
所述耐高温塑料薄膜市场上可得,要求双镜面、热变形温度180℃。
所述硅胶辊5,采用液体硅胶加800目金刚砂,制作成硬度为80HS的液体硅胶辊;所述镜面辊6与镜面辊7表面硬度为HRC62、辊筒表面光洁度为Ra0.01(光洁度14级)。
实施例2
一种PMMA超薄超透薄膜,由90KG PMMA、8KG甲基丙烯酸甲酯-丁二烯-甲基丙烯酸脂共聚物、2KG聚乙烯接枝马来酸酐PE-g-MAH原料组分组成。
其制备方法为:
将上述各原料组分进行混合,得到混合物;将混合物加入造粒机的搅拌室中,造粒机采用同向平行双螺杆,螺杆直径20mm,螺杆长径比32:1,造粒温度180℃,通过造粒机制成颗粒;如图1所示,将所述颗粒经充分干燥后通过单螺杆挤出机1熔融挤出,由挤出机模头9进入压延装置2压延,耐高温塑料薄膜覆膜设备4设有薄膜张力调节装置10,用于向硅胶辊5提供耐高温塑料薄膜进行贴合形成镜面,PMMA超薄超透薄膜经挤出机模头9挤出,进入胶辊5与镜面辊6之间进行镜面抛光,然后进入镜面辊6与镜面辊7之间进一步镜面抛光成型,经冷却辊组8冷却导出,进入成品收卷装置3收卷,制作出厚度为0.05mm的超薄、超透薄膜。原料粒子干燥温度120℃,干燥时长4h,;挤出机螺杆温度220℃,输送段温度230℃,挤出压力5MPa;压延生产速度30m/min。
所述耐高温塑料薄膜市场上可得,要求双镜面、热变形温度180℃。
所述硅胶辊5,采用液体硅胶加800目金刚砂,制作成硬度为80HS的液体硅胶辊;所述镜面辊6与镜面辊7表面硬度为HRC62、辊筒表面光洁度为Ra0.01(光洁度14级)。
实施例3
一种PMMA超薄超透薄膜,由90KG PMMA、6KG甲基丙烯酸甲酯-丁二烯-甲基丙烯酸脂共聚物、4KG聚乙烯接枝马来酸酐PE-g-MAH原料组分组成。
其制备方法为:
将上述各原料组分进行混合,得到混合物;将混合物加入造粒机的搅拌室中,造粒机采用同向平行双螺杆,螺杆直径20mm,螺杆长径比35:1,造粒温度190℃,通过造粒机制成颗粒;如图1所示,将所述颗粒经充分干燥后通过单螺杆挤出机1熔融挤出,由挤出机模头9进入压延装置2压延,耐高温塑料薄膜覆膜设备4含有薄膜张力调节装置10,用于向硅胶辊5提供耐高温塑料薄膜进行贴合形成镜面,PMMA超薄超透薄膜经挤出机模头9挤出,进入胶辊5与镜面辊6之间进行镜面抛光,然后进入镜面辊6与镜面辊7之间进一步镜面抛光成型,经冷却辊组8冷却导出,进入成品收卷装置3收卷,制作出厚度为0.05mm的超薄、超透薄膜。原料粒子干燥温度120℃,干燥时长4h,;挤出机螺杆温度230℃,输送段温度240℃,挤出压力10MPa;压延生产速度20m/min。
所述耐高温塑料薄膜市场上可得,要求双镜面、热变形温度180℃。
所述硅胶辊5,采用液体硅胶加800目金刚砂,制作成硬度为80HS的液体硅胶辊;所述镜面辊6与镜面辊7表面硬度为HRC62、辊筒表面光洁度为Ra0.01(光洁度14级)。
实施例4
一种PMMA超薄超透薄膜,由90KG PMMA,7KG甲基丙烯酸甲酯-丁二烯-甲基丙烯酸脂共聚物、3KG聚乙烯接枝马来酸酐PE-g-MAH原料组分组成。
其制备方法为:
将上述各原料组分进行混合,得到混合物;将混合物加入造粒机的搅拌室中,造粒机采用同向平行双螺杆,螺杆直径20mm,螺杆长径比35:1,造粒温度190℃,通过造粒机制成颗粒;如图1所示,将所述颗粒经充分干燥后通过单螺杆挤出机1熔融挤出,由挤出机模头9进入压延装置2压延,耐高温塑料薄膜覆膜设备4含有薄膜张力调节装置10,用于向硅胶辊5提供耐高温塑料薄膜进行贴合形成镜面,PMMA超薄超透薄膜经挤出机模头9挤出,进入胶辊5与镜面辊6之间进行镜面抛光,然后进入镜面辊6与镜面辊7之间进一步镜面抛光成型,经冷却辊组8冷却导出,进入成品收卷装置3收卷,制作出厚度为0.05mm的超薄、超透薄膜。原料粒子干燥温度90℃,干燥时长5h,;挤出机螺杆温度230℃,输送段温度240℃,挤出压力10MPa;压延生产速度20m/min。
所述耐高温塑料薄膜市场上可得,要求双镜面、热变形温度180℃。
所述硅胶辊5,采用液体硅胶加800目金刚砂,制作成硬度为80HS的液体硅胶辊;所述镜面辊6与镜面辊7表面硬度为HRC62、辊筒表面光洁度为Ra0.01(光洁度14级)。
性能检测:
将上述实施例1-4制成品PMMA超薄超透薄膜按《GBT 18833-2012道路交通反光膜》中的检测方法及标准进外观质量、耐化学性、耐候性、耐温性检测,经检测符合以下标准:
1.外观质量:外观表面平滑、洁净,无明显颗粒、划痕、条纹等外观缺陷;
2.耐高低温性能:经耐高低温试验后无明显变形,无裂缝;
3.耐溶剂性:经汽油和乙醇浸泡后无溶解;
4.耐盐雾腐蚀性能:无变色、侵蚀;
5.耐候质量:无侵蚀、粉化等损坏。
表一为本发明PMMA超薄超透薄膜的各原料组分及其用量范围以及所起的作用,在该表述范围内均可实现本发明的目的。表二及表三为本发明的工艺名称及具体的工艺要求,在所述参数范围内均可实现本发明的目的。
表一
表二
表三
尽管结合优选实施方案具体展示和介绍了本发明,但所属领域的技术人员应该明白,在不脱离所附权利要求书所限定的本发明的精神和范围内,在形式上和细节上可以对本发明做出各种变化,均为本发明的保护范围。
Claims (2)
1.一种双镜面压延的PMMA超薄超透薄膜的制作方法,其特征在于,包括以下步骤:
(1)原料混合:将聚甲基丙烯酸甲酯85~95份、增韧剂5~8份、相容剂2~5份投入高速混合机内高速搅拌10min~15min,搅拌温度控制在60℃~70℃,得到混合物,经冷混机将混合物温度降至40℃~50℃;所述增韧剂为甲基丙烯酸甲酯-丁二烯-甲基丙烯酸酯共聚物,所述相容剂为聚乙烯接枝马来酸酐;所述聚甲基丙烯酸甲酯选自三菱、住友或奇美普通级聚甲基丙烯酸甲酯;
(2)造粒:将步骤(1)制得的混合物经同向平行双螺杆造粒机改性造粒,得到原料粒子,所述同向平行双螺杆的直径20~25mm,螺杆长径比32:1~52:1,造粒温度180℃~200℃;
(3)挤出压延:将步骤(2)制得的原料粒子干燥后由挤出压延设备压延成型,制作出厚度为0.05mm~0.08mm的热熔胶薄膜,所述原料粒子干燥温度控制在80℃~100℃,干燥时长控制在4h~6h;挤出单螺杆温度控制在220℃~240℃,输送段温度控制在230℃~250℃,挤出压力5MPa~12MPa,生产速度为5m/min~30m/min;
(4)成品收卷;
步骤(3)中所述挤出压延设备包括依次排列的单螺杆挤出机(1)、压延设备(2)、成品收卷装置(3),所述压延设备(2)包括依次排列的耐高温塑料薄膜覆膜设备(4)、硅胶辊(5)、第一镜面辊(6)、第二镜面辊(7)、冷却辊组(8),硅胶辊(5)和第一镜面辊(6)之间缝隙正上方设有挤出机模头(9);所述硅胶辊(5)采用液体硅胶加800目金刚砂,制作成硬度为80HS的液体硅胶辊,所述第一镜面辊(6)、第二镜面辊(7)的表面硬度为HRC62、辊筒表面光洁度为Ra0.01,光洁度14级;所述耐高温塑料薄膜为双镜面、热变形温度180℃的耐高温塑料薄膜。
2.根据权利要求1所述的一种双镜面压延的PMMA超薄超透薄膜的制作方法,其特征在于:所述耐高温塑料薄膜覆膜设备(4)上设有薄膜张力调节装置(10)。
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