CN106827847B - 热敏记录材料 - Google Patents

热敏记录材料 Download PDF

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CN106827847B
CN106827847B CN201611042555.8A CN201611042555A CN106827847B CN 106827847 B CN106827847 B CN 106827847B CN 201611042555 A CN201611042555 A CN 201611042555A CN 106827847 B CN106827847 B CN 106827847B
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polymer particles
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spherical polymer
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CN106827847A (zh
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B·R·艾因斯拉
V·V·金兹伯格
L·李
J·A·罗珀三世
R·史密斯
J·杨
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Dow Global Technologies LLC
Rohm and Haas Co
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Abstract

本发明涉及一种热敏记录材料，其包含纸、安置于所述纸上的底涂层和安置于所述底涂层上的热敏记录层，其中所述底涂层包含粘合剂以及第一和第二中空球形聚合物粒子，其中所述第一中空球形聚合物粒子具有在1.2μm到1.8μm范围内的直径；所述第二中空球形聚合物粒子具有在0.25μm到1.0μm范围内的直径；所述第二与所述第一中空球形聚合物粒子的数目比在1:1到20:1范围内；所述第二中空球形聚合物粒子的直径在所述第一中空球形聚合物粒子的直径的15％到65％范围内；所述第一中空球形聚合物粒子的干容积密度在0.25到0.5g/mL范围内；且所述第二中空球形聚合物粒子的干容积密度在0.30到0.90g/mL范围内。

Description

热敏记录材料
技术领域
本发明涉及包含安置于纸上的底涂层，和安置于底涂层上的热敏记录层的热敏记录材料。
背景技术
已知使用用于热敏记录材料的底涂层防止油墨非所要地吸收到纸中且对纸提供热绝缘。因此，涂布纸比未涂布纸产生更清晰更明亮图像且具有更好反射性。
US 6,531,183公开包含粘合剂和中空颜料粒子以改良纸的光泽度的涂料组合物。涂料组合物可任选地包含第二颜料粒子，其可为固体或“有液泡的”且可与第一粒子的尺寸相同或不同。
US 6,780,820公开多种底涂层，包括含有用于超临界颜料体积浓度涂层中的无机颜料、精细有机单一空隙化粒子或多空隙化粒子的那些。
US 8,334,047公开来源于包含粘合剂和双峰分布的第一和第二中空聚合颜料的组合物的底涂层的用途，所述颜料具有无酸亲水性核心和一般在300到1,100nm范围内的体积平均直径。
发现适用作提供纸涂层强度与涂布有底涂层和热敏记录层的印刷纸的光学密度的平衡的底涂层的材料将为底涂组合物技术领域中的进步。
发明内容
在第一方面中，本发明为包含粘合剂以及具有水性中和酸核心的第一和第二核-壳聚合物粒子的水性分散液的涂料组合物，其中
a)第一核-壳聚合物粒子具有在1.0μm到1.8μm范围内的直径；
b)第二核-壳聚合物粒子具有在0.25μm到1.0μm范围内的直径；
c)第二与第一核-壳聚合物粒子的数目比在1:1到20:1范围内；
d)第二核-壳聚合物粒子的直径在第一核-壳聚合物粒子的直径的15％到65％范围内；
e)第一核-壳聚合物粒子的干容积密度在0.25到0.5g/mL范围内；且
f)第二核-壳聚合物粒子的干容积密度在0.30到0.90g/mL范围内。
在第二方面中，本发明为包含纸、安置于纸上的底涂层和安置于底涂层上的热敏记录层的热敏记录材料，其中底涂层包含粘合剂和双峰分布的第一和第二中空球形聚合物粒子，其中
a)第一中空球形粒子具有在1.0μm到1.8μm范围内的直径；
b)第二中空球形粒子具有在0.25到1.0μm范围内的直径；
c)第二与第一中空球形聚合物粒子的数目比在1:1到20:1范围内；
d)第二核-壳聚合物粒子的直径在第一核-壳聚合物粒子的直径的15％到65％范围内；
e)第一中空球形聚合物粒子的干容积密度在0.25到0.5g/mL范围内；且
f)第二中空球形粒子的干容积密度在0.30到0.90g/mL范围内。
本发明通过提供适用作对于热敏记录材料应用显示改进的强度和改进的光学密度的底涂层的组合物满足所属领域中的需要。
具体实施方式
在第一方面中，本发明为包含粘合剂以及具有水性中和酸核心的第一和第二核-壳聚合物粒子的水性分散液的涂料组合物，其中
a)第一核-壳聚合物粒子具有在1.0μm到1.8μm范围内的直径；
b)第二核-壳聚合物粒子具有在0.25μm到1.0μm范围内的直径；
c)第二与第一核-壳聚合物粒子的数目比在1:1到20:1范围内；
d)第二核-壳聚合物粒子的直径在第一核-壳聚合物粒子的直径的15％到65％范围内；
e)第一核-壳聚合物粒子的干容积密度在0.25到0.5g/mL范围内；且
f)第二核-壳聚合物粒子的干容积密度在0.30到0.90g/mL范围内。
粘合剂为涂料组合物的成膜组分且不限制其范围。粘合剂的实例包括聚合粘合剂，如聚丙烯酸树脂、聚乙酸乙烯酯、(聚)乙烯基-丙烯酸树脂、(聚)苯乙烯-丙烯酸树脂、(聚)苯乙烯-丁二烯、(聚)乙酸乙烯酯/乙烯、(聚)乙烯基-丙烯酸树脂、聚氨基甲酸酯、聚丙烯酰胺、聚乙烯醇和聚酯。按组合物的重量计，用于本发明组合物的粘合剂的重量分率通常在2到50，更优选地30重量％的范围内。
组合物进一步包含具有水性中和酸核心的第一和第二核-壳聚合物粒子。这些粒子称为中空球形粒子或不透明聚合物且可通过所属领域中已知的方法制备。(参见例如US6,020,435)。
第一核-壳聚合物粒子具有在1.0μm、优选地1.2μm、更优选地1.3μm且最优选地1.4μm到1.8μm、优选地1.7μm且更优选地1.6μm范围内的直径。第二核-壳聚合物粒子具有在0.25μm、优选地0.3μm、更优选地0.35μm且最优选0.4μm到1μm、优选地0.8μm、更优选地0.6μm且最优选0.5μm范围内的直径。
就具有500nm到1μm的粒度的a)第一核-壳聚合物粒子和b)第二核-壳聚合物粒子来说的粒径按照定义为通过使用具有1.63数值孔径的100×油浸镜头的Leica光学显微镜测量的直径；每一直径读取通过筛选经过粒子中心的最大距离的边到边距离的读数进行且经至少10个粒子取平均值。
具有250nm到小于500nm的粒度的第二核-壳聚合物粒子的粒径按照定义为使用BI90Plus粒度分析仪测量的直径。
第一核-壳聚合物粒子的特征进一步在于在0.25、优选地0.30、更优选地0.35g/mL到0.5、优选地0.45并且更优选地0.40g/mL范围内的干容积密度。适用作第一核-壳聚合物粒子的水性分散液的商业产品的实例为ROPAQUETM TH-2000不透明聚合物(陶氏化学公司(The Dow Chemical Company)或其附属公司的商标)。根据US 6,020,435第16栏、第10-67行到第17栏、第1-7行中公开的程序测量干容积密度。
第二核-壳聚合物粒子的特征进一步在于在0.30、优选地0.40、更优选地0.50且最优选地0.55g/mL到0.90、优选地0.80、更优选地0.75且最优选地0.65g/mL范围内的干容积密度。适用作第二核-壳聚合物粒子的水性分散液的商业产品的实例为ROPAQUETM ULTRA E不透明聚合物。
第二与第一核-壳聚合物粒子的数目比在1:1、优选地2:1、更优选地3:1且最优选4:1到20:1、优选地15:1、更优选地12:1且最优选地10:1范围内。
第二核-壳聚合物粒子的直径在第一核-壳聚合物粒子的直径的15％、优选地20％、更优选地25％、最优选地27％到65％、优选地40％、更优选地33％且最优选地30％范围内。举例来说，如果第一核-壳聚合物粒子具有1.5μm的直径且第二核-壳聚合物粒子具有425nm的直径，那么第二核-壳聚合物粒子的直径为第一核-壳聚合物粒子的直径的0.425/1.5或28.3％。
当组合物以膜形式施用时，第一和第二核-壳聚合物浓度的总颜料容积浓度(PVC)通常在50％到98％、优选地95％范围内。优选地，膜的PVC为超临界的。已发现可在超临界PVC下制备具有出人意料的强度的底涂层。
本发明组合物可包括其它无机或聚合颜料，如碳酸钙、煅烧高岭土、TiO2、ZnO、Al(OH)3、BaSO4和SiO2，但可在不存在辅助颜料的情况下实践。组合物还可包括其它添加剂，如消泡剂、交联剂、表面活性剂和热熔性材料，但可在不存在辅助添加剂的情况下实践。
本发明的涂料组合物适用作安置于纸上的热敏记录层的底涂层(中间第一层)。因此，在第二方面中，本发明为包含纸、安置于纸上的底涂层和安置于底涂层上的热敏记录层的热敏记录材料，其中底涂层包含粘合剂以及第一和第二中空球形聚合物粒子，其中第一中空球形聚合物粒子具有在1.0μm、优选地1.2μm、更优选地1.3μm且最优选1.4μm到1.8μm、优选地1.7μm且更优选地1.6μm范围内的直径；其中第二中空球形聚合物粒子具有在0.25、优选地0.3μm、更优选地0.35μm且最优选地0.4μm到1μm、优选地0.8μm、更优选地0.6μm且最优选地0.5μm范围内的直径；其中第二与第一中空球形聚合物粒子的数目比在1:1、优选地2:1、更优选地3:1且最优选地4:1到20:1、优选地15:1且更优选地12:1范围内；且其中第二中空球形聚合物粒子的直径在第一中空球形聚合物粒子的直径的15％、优选地20％、更优选地25％、最优选地27％到65％、优选地40％、更优选地33％且最优选地30％范围内。
第一中空球形聚合物粒子的特征进一步在于在0.25、优选地0.30、更优选地0.35g/mL到0.5、优选地0.45并且更优选地0.40g/mL范围内的干容积密度。第二中空球形聚合物粒子的特征进一步在于在0.30、优选地0.40、更优选地0.50且最优选地0.55g/mL到0.90、优选地0.80、更优选地0.75且最优选地0.65g/mL范围内的干容积密度。
底涂层可通过如辊涂覆器、湿式涂覆器、帘式涂布机或喷射方法的多种方法中的任一者涂覆到纸上。底涂层可通过包括刮刀、气刀、光杆、螺纹棒或绕线棒的多种方法中的任一者平滑化。底涂层的最终干涂层重量通常在1、更优选地2g/m2到25、更优选地10且最优选6g/m2范围内。
通常包含隐色染料(参见美国专利4,929,590)的热敏记录层接着涂覆于底涂层上方，厚度通常在1g/m2到20g/m2、更优选地10g/m2范围内。热敏记录层还可包含多种其它添加剂，包括粘合剂、填充剂、交联剂、表面活性剂和热熔性材料。
实例
实例1-制备双峰中空颜料调配物
ROPAQUETM TH-2000不透明聚合物浆料(1.5μm直径，151.8g，31.9g干燥重量，干容积密度0.36g/mL，空隙率65％)在搅拌下添加到容器中，接着添加ROPAQUE ULTRA E不透明聚合物浆料(0.4μm直径，3.07g，0.95g干燥重量，干容积密度0.58g/mL，空隙率45％)，接着添加RHOPLEXTM P-308苯乙烯-丙烯酸粘合剂(30.47g，15.16g干燥重量，13.5％体积分率)，接着添加聚乙烯醇(13.45g，1.95g干燥重量，1.5％体积分率)，接着添加水(1.2g)以形成具有25.0重量％固体含量的水性悬浮液。由调配物制备的干燥涂层的PVC为85％(其中TH-2000占83.4％且ULTRA E占1.6％)且TH2000与ULTRA E的数目比为约1:1。
如下计算每克干燥颜料的粒子数目：通过首先计算单一粒子的体积(V)且接着使用颜料粒子的已知干容积密度(d)将体积转化为质量以获得单一粒子的质量：
V＝4/3πr3
m＝V×d
每克的粒子数目仅为1/m。使用此方法，如下计算ULTRA E与TH-2000的数目比：
5.15×1013个粒子/克ULTRA E×0.95g ULTRA E＝4.9×1013个ULTRA E粒子
1.57×1012个粒子/克TH-2000×31.9g TH-2000＝5.0×1013个TH-2000粒子
ULTRA E:TH-2000约1:1
如表1中所示改变颜料量制得一系列调配物。对于实例2-11和C2，干燥涂层的总PVC为87.5％，其中粘合剂和聚乙烯醇保持相同，占剩下的12.5％。调节水添加以维持约25％的固体含量。ULTRA E#分率是指ULTRA E相对于TH-2000的数目分率。体积分率是指ULTRA E相对于TH-2000的体积分率。C1-C3係指比较实例1-3。
表1-ULTRA E相对于TH-2000的数目分率和体积分率
实例编号 ULTRA E#分率 ULTRA E与TH-2000的比率 体积分率
C1 0 0:1 0
1 0.5 1:1 0.02
2 0.67 2:1 0.04
3 0.75 3:1 0.05
4 0.8 4:1 0.07
5 0.83 5:1 0.09
6 0.86 6:1 0.10
7 0.88 7:1 0.12
8 0.89 8:1 0.13
9 0.9 9:1 0.15
10 0.91 10:1 0.16
11 0.99 100:1 0.65
C2 0.999 1000:1 0.95
C3 1 - 1
调配物用于形成如以下部分中所述的底涂层。
制备底涂层
样品如下涂布于纸上：9"×12"纸张(重量72g/m2)置于下引机上且在顶部上用夹子固定。跨越待涂布的纸顶部涂覆一条透明胶带以防止随后涂覆的涂层从纸浸出。绕线棒跨越纸顶部置于胶带上方，且涂料珠粒使用滴管而跨越纸置于胶带上。棒沿纸向下移动以均匀地涂布所述纸以形成底涂层(重量约4到4.5g/m2)。涂布的纸张置于一张卡纸板上且在80℃下干燥1min，接着自烘箱移开且使其在设定为22℃和50％相对湿度的受控温度和湿度房间(CTR)中平衡2h。
涂层强度测量
涂层强度根据ASTM T-499su-64用IGT可印刷性测试仪测量。测试结果就粘度-速度乘积(IGT-VVP)来说进行报导，其为涂层强度的量度。表2显示小不透明聚合物(ULTRA E)的数目分率与涂层强度(如通过IGT-VVP体现)之间的关系。
表2-作为ULTRA E数目分率的函数的IGT-VVP
实例编号 ULTRAE#分率 ULTRAE与TH-2000的比率 IGT-VVP
C1 0 0:1 7
1 0.5 1:1 11
2 0.67 2:1 16
3 0.75 3:1 17
4 0.80 4:1 36
5 0.83 5:1 28
6 0.86 6:1 36
7 0.88 7:1 36
8 0.89 8:1 38
9 0.90 9:1 40
10 0.91 10:1 40
11 0.99 100:1 11
C2 0.999 1000:1 8
C3 1 - 8
结果展示双峰调配物改进涂层强度，其中最大改进出现于0.80到0.95的ULTRA E数目分率范围。
制备热印刷层
底涂纸样品大体上使用用于制备底涂层的程序涂布有约3.5g/m2含有隐色染料和显影剂的热成像材料。
光学密度测量
经涂布的纸根据ASTM F1405-98(2013)印刷；使用Atlantek纸测试仪型号200。使用Atlantek热敏印刷机的印刷条件如下：50％棋盘图案，序列点脉冲持续时间至多0.8ms，Tcycle＝5.000ms。在21.5V的施加电压下，印刷头电阻为629欧姆。使用X-Rite 428手持型分光光密度计在每点0.4mJ下测量涂布纸的经印刷热纸光学密度。
表3说明小不透明聚合物(ULTRA E)的数目分率对OD印刷光学密度的影响。
表3-作为ULTRA E数目分率的函数的印刷光学密度
Figure BDA0001160747950000061
Figure BDA0001160747950000071
数据显示可通过将ULTRA E分率调节到约0.67到约0.91的范围实现IGT-VVP强度和光学密度的平衡。
制备非中空聚苯乙烯珠粒
如下制备三批具有不同直径的非中空聚苯乙烯珠粒的水性分散液以展示粒度比率对涂层强度的影响。
制备200nm聚苯乙烯珠粒(PS1)
装备有机械搅拌器和回流冷凝器的4颈圆底烧瓶以去离子水(1535g)填充且加热到92℃。向此烧瓶中添加过硫酸铵(4g，于90g水中)和种子乳胶(104.5g，41％固体，60nm)。经120min添加含有去离子水(815g)、十二烷基苯磺酸钠(25.5g，22.5％固体)、苯乙烯(1256g)和甲基丙烯酸(38.87g)的单体乳液。过硫酸铵溶液(2g，于120g水中)与单体乳液进料并流。在反应过程期间，温度维持于88℃。在完成进料之后，经15min添加额外量的过硫酸铵溶液(0.5g，于30g水中)。反应物接着冷却到75℃且馈入硫酸亚铁溶液(32.4g，0.15％活性)。残余单体通过馈送叔丁基氢过氧化物(0.80g，于25g水中)和异抗坏血酸(1.10g，于25g水中)溶液还原。所得分散液具有32.4％的固体含量和187nm的粒度。
制备300nm聚苯乙烯珠粒(PS2)
300nm珠粒大体上如关于制备200nm珠粒所描述制备，不同之处在于种子乳胶(105.4g，45％固体，100nm)。所得分散液具有31.8％的固体含量和286nm的粒度。
制备400nm聚苯乙烯珠粒(PS3)
400nm珠粒大体上如关于制备200nm珠粒所描述制备，不同之处在于种子乳胶(133.7g，32％固体，143nm)。所得分散液具有31.7％的固体含量和407nm的粒度。
粒度比率影响
发现粒度比率对涂层强度具有显著影响，其可使用中空或非中空球体测量。表3显示第二(较小)聚合物粒子的粒径对IGT-VVP的影响。在这些实验中的每一个中，第一(较大)聚合物粒子为1.5μm，PVC为87.5％，且小粒子数目分率为0.91。名称是指小聚合物粒子的分散液的名称；OP-96是指ROPAQUETM OP-96不透明聚合物；AF-1055是指ROPAQUETM AF-1055不透明聚合物(陶氏化学公司或其附属公司的商标)。苯乙烯1、2和3全部为如上文所述制备的非中空球形珠粒。比率是指小粒径与大粒径的比率。
表4-粒度比率对涂层强度的影响
小粒径(μm) 名称 比率 IGT-VVP
1 AF-1055 0.67 8
0.5 OP-96 0.33 32
0.42 ULTRA E 0.28 36
0.41 PS1 0.27 29
0.29 PS2 0.19 15
0.19 PS3 0.13 12
结果展示在约0.28的小粒子与大粒子的比率下形成最强涂层。

Claims (6)

1.一种热敏记录材料，其包含纸、安置于所述纸上的底涂层和安置于所述底涂层上的热敏记录层，其中所述底涂层包含粘合剂以及第一中空球形聚合物粒子和第二中空球形聚合物粒子，其中：
a）所述第一中空球形聚合物粒子具有在1.4 μm到1.6 μm范围内的直径；
b）所述第二中空球形聚合物粒子具有在0.4到0.5 μm范围内的直径；
c）所述第二中空球形聚合物粒子与所述第一中空球形聚合物粒子的数目比在4:1到10:1范围内；
d）所述第二中空球形聚合物粒子的直径在所述第一中空球形聚合物粒子的直径的27%到30%范围内；
e）所述第一中空球形聚合物粒子的干容积密度在0.25到0.5 g/mL范围内；且
f）所述第二中空球形聚合物粒子的干容积密度在0.30到0.90 g/mL范围内。
2.根据权利要求1所述的热敏记录材料，其中所述第一中空球形聚合物粒子的干容积密度在0.30到0.45 g/mL范围内；且所述第二中空球形聚合物粒子的干容积密度在0.40到0.80 g/mL范围内。
3.根据权利要求1所述的热敏记录材料，其中所述第一中空球形聚合物粒子的干容积密度在0.35到0.40 g/mL范围内；且所述第二中空球形聚合物粒子的干容积密度在0.50到0.75 g/mL范围内。
4.根据权利要求1所述的热敏记录材料，其中所述第一中空球形聚合物粒子的干容积密度在0.35到0.40 g/mL范围内；且所述第二中空球形聚合物粒子的干容积密度在0.55到0.65 g/mL范围内。
5.根据权利要求1所述的热敏记录材料，其中所述底涂层的干涂层厚度在1到25 g/m2范围内，且所述记录层的厚度在1 g/m2到20 g/m2范围内。
6.根据权利要求1所述的热敏记录材料，其中所述底涂层的干涂层厚度在2到6 g/m2范围内，且所述记录层的厚度在1 g/m2到10 g/m2范围内。
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