CN108221474A - 一种新型造纸施胶剂的制备方法 - Google Patents
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Abstract
一种新型造纸施胶剂的制备方法,属于造纸施胶剂的技术领域,包括以下步骤:A、按重量份数计,取硬脂酸60‑80份,二乙醇胺2‑3份,二乙烯三胺6‑14份,于140‑220℃反应4‑6h,降温,得到反应料液,备用;B、按重量份数计,取水100份,淀粉2‑10份,混合、糊化后,降温至50℃,得糊化淀粉液,或取水100份,高分子聚合物0.5‑10份,混合、升温至50℃,得混合液;向糊化淀粉液或混合液中加入步骤A所得反应料液5‑14份,加入复合表面活性剂0.2‑1份,滴加环氧氯丙烷3‑10份,升温至70℃,保温反应2‑5小时,加水5份,降温,得到造纸施胶剂。本发明制备方法简单、易操作,制备过程反应温和稳定,制备的施胶剂施胶效果好,防潮效果更好,更适应当前废纸浆造纸的需要。
Description
技术领域
本发明属于造纸施胶剂的技术领域,设计了一种新型的造纸施胶剂-阳离子硬酯酰胺乳液,具体涉及一种新型的造纸施胶剂的制备方法。本发明制备方法简单、易操作,制备过程反应温和稳定,采用本发明方法制备的施胶剂施胶效果好,防潮效果更好,且所制备的施胶剂对增强纤维之间的结合力起一定作用,更适应当前废纸浆造纸的需要。
背景技术
施胶剂是重要的湿部化学品,我国现今对造纸施胶剂进行大幅度的开发应用,上世纪八十年代以前大多采用皂化松香施胶剂和用马来酸酐加成制得的强化松香施胶剂,其只要品种有松香胶、强化松香胶和阴离子分散松香胶和阳离子分散松香胶等。这一类施胶剂属于酸性施胶,在使用过程中加入大量的硫酸铝,主要应用在浆内施胶,给设备和管道造成腐蚀。并且纸张返黄易脆。
中性施胶技术在我国是在上世纪八十年代开始研究,八十年代末开始使用九十年代中期推广开来,到现在已经广泛使用,已经成为主流的浆内施胶剂和表面施胶剂。中性施胶剂主要有AKD(烷基烯酮二聚体)乳液、聚氨酯乳液、丙烯酸树脂乳液和苯乙烯与马来酸酐共聚物或其余多乙撑多胺反应制得的阳离子化聚合物、苯乙烯丙烯酸酯共聚物乳液等。其中AKD(烷基烯酮二聚体)乳液由于使用成本低,使用的PH值范围宽等特点,成为目前造纸工业中最广泛的中性施胶剂。
AKD蜡是由硬脂酸经过酰化制成硬酯酰氯,再在有机溶剂中进行烯酮化和二聚体。反应产物为40℃-50℃的蜡状物。
AKD分子与纤维的羟基反应生β-酮酯,并固着在纤维表面上,疏水性的烷基向外,从而获得疏水性。然而AKD也和水反应生成不稳定的β-酮酸,即为水解产物,不利于抗水。其在一般情况下在30℃搅拌30分钟,约有15%左右的发生水解,尤其是在70℃-80℃表面施胶的环境中,水解速度更快,约有50%以上水解。AKD与纤维间的酯化反应是在足够的温度和时间情况下反应的,这样有熟化期。在实际的生产应用中,带来诸多不便,会出现假施胶或者达不到预期的抗水效果。另外由于AKD蜡本身熔点低,在抗热水,防潮效果差。另外因生产过程需要酰化,使用光气,产物伴随有废酸的产生,给环境和安全造成潜在的危害性大。在国家环保和安全的紧迫要求下,在随着造纸工艺由浆内施胶逐渐转成表面施胶的情况下,AKD不能满足当前的需要。因此研发新型的阳离子造纸施胶剂是目前需要解决的问题。
发明内容
本发明为研发施胶效果好的新型造纸施胶剂,提供了一种新型的造纸施胶剂的制备方法,制备了一种阳离子硬酯酰胺乳液,具有良好的自留着性、施胶度良好。
本发明为实现其目的采用的技术方案是:
一种新型造纸施胶剂的制备方法,包括以下步骤:
A、按重量份数计,取硬脂酸60-80份,二乙醇胺2-3份,二乙烯三胺6-14份,于140-220℃反应4-6h,降温至110-120℃,得到反应料液,备用;
B、按重量份数计,取水100份,淀粉2-10份,混合、糊化后,降温至45-50℃,得糊化淀粉液,或取水100份,高分子聚合物0.5-10份,混合、升温至50℃,得混合液;向糊化淀粉液或混合液中加入步骤A所得反应料液5-14份,加入复合表面活性剂0.2-1份,滴加环氧氯丙烷3-10份,升温至70-75℃,保温反应2-5小时,加水4-6份,降温至室温,得到白色乳液即为造纸施胶剂。
步骤B中的淀粉选自经过阳离子化或者氧化后的玉米淀粉或木薯淀粉。
将步骤B中的水和淀粉混合后,于90-95℃糊化45-60min。
步骤B中的高分子聚合物为具有1000至10万低分子分子量、阳电荷密度大的多胺型聚合物。
高分子聚合物选自聚酰胺环氧氯丙烷树脂、聚乙烯亚胺、阳离子聚丙烯酰胺、聚二甲基二烯丙基氯化铵中的一种或几种组合。
所述的复合表面活性剂包括非离子型表面活性剂和阳离子型表面活性剂。
非离子型表面活性剂选自聚氧乙烯醚类表面活性剂或聚氧乙烯脂肪酸酯,HLB值要求在10-15之间。例如烷基酚类聚氧乙烯醚,OP-10,OP-12,吐温系列或者司盘系列T-40,T-60,S-85等。
阳离子表面活性剂为具有碳链在10-18之间的、HLB值在15-17的烷基季胺盐类的阳离子表面活性剂。例如十六烷基三甲基溴化铵或十六烷基三甲基氯化铵。
本发明的有益效果是:
本发明制备方法简单,制备过程反应温和稳定,制备得到的硬酯酰胺乳液作为新型施胶剂具有良好的自留着性,防水性好,施胶效果良好,抗热水效果和防潮效果更好,且所制备的施胶剂对增强纤维之间的结合力起一定作用,更适应当前废纸浆造纸的需要。在极低的施胶量下即可产生所需的施胶效果,相对于现有施胶剂大大减少的施胶剂用量。本发明制备的造纸施胶剂储存时间长,存放干燥处保质期达22个月以上,且储存过程中产品性能稳定。
采用本发明制备的造纸施胶剂对纸张进行表面施胶处理,不仅可以增加纸张的抗水性,还可提高纸张的物理强度、赋予纸张抗酸碱性;施胶于纸张表面还可改善纸面平滑度、印刷性能、表面强度、纸张挺度及耐破防水、更有利于抗返潮、使纸张的存放期更长。
本发明施胶剂具有施胶稳定,没有熟化期,防潮性好的优势;在生产过程中,采用乳液聚合的方法,在油水相界面上反应,边反应边乳化,反应过程易控制,形成粒度小的微乳液。
本发明在硬脂酸与二乙烯三胺反应的过程中加入了二乙醇胺。由于硬脂酸与二乙烯三胺反应生成双硬酯酰胺其熔点在120℃以上,其在水中反应和乳化带来难度,为解决该难度,本发明通过加入二乙醇胺后,形成双硬脂酸酯和双硬质酰胺的混合物,这样降低了乳化和反应的难度,同时在硬脂酸和二乙烯三胺中加入二乙醇胺对于防潮和抗热水性能提高了。
本发明采用高分子聚合物或淀粉做反应中的分散剂,使产品稳定性能提高,又增加了纸张纤维间的结合力,并适应当前废纸浆造纸。
本发明通过加入淀粉或高分子聚合物,对阳离子硬酯酰胺形成阳离子后起到分散作用,防止自身的阳离子硬脂酸酯经过碰撞后进行缔合,形成大颗粒,对乳液起到稳定性能,或者叫做胶体保护性能。同时由于淀粉和高分子聚合物的加入,有空间位阻,以至于在季胺化反应中,温度在70℃-75℃反应过程是可控,温和的反应。否则,在70℃-75℃下反应,会迅速出现交联,形成网状结构。
随着涂布损纸,脱墨废纸、高得率浆等废纸使用及白水循环封闭使用,纸机湿部干扰物质,特别是水中溶解性物质和胶体物质溶度越来越高,这些里面含有大量的阴离子垃圾,从而导致加入的阳离子物质的效能大大减少,甚至失去效果,面对该问题,本发明通过加入阳离子淀粉或者阳离子高分子聚合物后,电荷密度高,迅速的与阴离子垃圾进行反应,保证了阳离子硬酯酰胺很好的结合,提高了其使用效果,因而在造纸应用中起到助留,增效作用。另外淀粉与高分子聚合物含有大量的羟基和氨基,易于纤维中的羟基形成氢键,有利于增强纸张的结合力,提高耐破和拉力。
步骤B的作用是形成自带有阳电荷的物质,同时因在复合表面活性剂和淀粉或高分子聚合物情况下进行乳化分散,形成一种稳定的,粒度在0.1-1.0微米白色均匀的乳液。其重要的控制参数,就是温度,当温度低于70℃时,易发生相变,由液态的分散液变成固态分散体,这样反应的粒度大,造成乳液不稳定,容易分层;如果高于75℃,阳离子化程度加快,反应加剧,会出现克服外在的双电层,破乳后进行交联反应。
本发明制备的施胶剂为中性施胶剂,且在应用过程中不需要加入硫酸铝,适应的pH值范围广。
本发明新型造纸施胶剂为阳离子硬酯酰胺乳液,由于其带有阳电荷,它能被纤维表面带的负电荷吸附后,自身的羟基或者氨基与纤维的表面的羟基形成牢固的离子键,或者是氢键,同时两个疏水性长链烷基伸向纤维表面,这样形成疏水,起到施胶作用。
具体实施方式
本发明的反应机理如下:
1)第一步反应:硬酯酰胺的生成和硬脂酸酯的生成
2CH3(CH2)16COOH+NH2(CH2)2NH(CH2)2NH2→(CH2)16CONH(CH2)2NH(CH2)2CO(CH2)16CH3+H2O2CH3(CH2)16COOH+Ho(CH2)2NH(CH2)2OH→CH3(CH2)16COOH(CH2)2NH(CH2)2COO(CH2)16CH3+H2O
2)第二步反应:阳离子化
这种自身具有阳电荷,与纤维自行固着后,两个长烷基链伸向外侧,形成疏水性。在此基团含酰胺键,羟基键,能很好的和纤维间的羟基形成氢键。下面结合具体实施例对本发明作进一步的说明。
一、具体实施例
实施例1
A、取硬脂酸60g,二乙醇胺2g,二乙烯三胺6g,于140℃反应6h,降温至110℃,得到反应料液,备用;
B、取水100g,阳离子玉米淀粉3g,混合后,于90℃糊化1h,降温至50℃,得糊化淀粉液,向糊化淀粉液中加入步骤A所得反应料液5g,加入复合表面活性剂0.2g,滴加环氧氯丙烷3g,升温至70℃,保温反应5小时,加水5g,降温至室温,得到白色乳液,即为造纸施胶剂。
其中复合表面活性剂为质量比为1:1的烷基酚类聚氧乙烯醚和十六烷基三甲基溴化铵。
实施例2
A、取硬脂酸70g,二乙醇胺3g,二乙烯三胺7g,于220℃反应4h,降温至120℃,得到反应料液,备用;
B、取水100g,聚酰胺环氧氯丙烷树脂10g,混合、升温至50℃,得混合液,向混合液中加入步骤A所得反应料液14g,加入复合表面活性剂1g,滴加环氧氯丙烷5g,升温至70℃,保温反应2小时,加水5g,降温至室温,得到白色乳液,即为造纸施胶剂。
其中复合表面活性剂为质量比为3:2的OP-10和十六烷基三甲氯化铵。
实施例3
A、取硬脂酸80g,二乙醇胺2.5g,二乙烯三胺8g,于180℃反应5h,降温至115℃,得到反应料液,备用;
B、取水100g,阳离子木薯淀粉6g,混合后,于90℃糊化1h,降温至45℃,得糊化淀粉液,向糊化淀粉液中加入步骤A所得反应料液7g,加入复合表面活性剂0.5g,滴加环氧氯丙烷7g,升温至70℃,保温反应2.5小时,加水5g,降温至室温,得到白色乳液,即为造纸施胶剂。
其中复合表面活性剂为质量比为2:3的T-40和十六烷基三甲氯化铵。
实施例4
A、取硬脂酸65g,二乙醇胺2.2g,二乙烯三胺9g,于1600℃反应4.5h,降温至118℃,得到反应料液,备用;
B、取水100g,聚乙烯亚胺0.5g,混合、升温至50℃,得混合液,向混合液中加入步骤A所得反应料液6g,加入复合表面活性剂0.3g,滴加环氧氯丙烷6g,升温至70℃,保温反应3小时,加水5g,降温至室温,得到白色乳液,即为造纸施胶剂。
其中复合表面活性剂为质量比为1:1的S-85和十六烷基三甲基溴化铵。
实施例5
A、取硬脂酸75g,二乙醇胺2.8g,二乙烯三胺10g,于150℃反应5.5h,降温至113℃,得到反应料液,备用;
B、取水100g,阳离子木薯淀粉2g,混合后,于90℃糊化1h,降温至48℃,得糊化淀粉液,向糊化淀粉液中加入步骤A所得反应料液8g,加入复合表面活性剂0.8g,滴加环氧氯丙烷9g,升温至70℃,保温反应4小时,加水5g,降温至室温,得到白色乳液,即为造纸施胶剂。
其中复合表面活性剂为质量比为1:1的T-60和十六烷基三甲基溴化铵。
实施例6
A、取硬脂酸63g,二乙醇胺2.3g,二乙烯三胺11g,于170℃反应5h,降温至115℃,得到反应料液,备用;
B、取水100g,阳离子聚丙烯酰胺5g,混合、升温至50℃,得混合液,向混合液中加入步骤A所得反应料液9g,加入复合表面活性剂0.7g,滴加环氧氯丙烷8g,升温至70℃,保温反应3.5小时,加水6g,降温至室温,得到白色乳液,即为造纸施胶剂。
其中复合表面活性剂为质量比为1:1的OP-12和十六烷基三甲基溴化铵。
实施例7
A、取硬脂酸68g,二乙醇胺2.7g,二乙烯三胺12g,于190℃反应5h,降温至110℃,得到反应料液,备用;
B、取水100g,阳离子玉米淀粉7g,混合后,于90℃糊化1h,降温至47℃,得糊化淀粉液,向糊化淀粉液中加入步骤A所得反应料液10g,加入复合表面活性剂0.6g,滴加环氧氯丙烷4g,升温至70℃,保温反应4.5小时,加水5g,降温至室温,得到白色乳液,即为造纸施胶剂。
其中复合表面活性剂为质量比为2:3的烷基酚类聚氧乙烯醚和十六烷基三甲基氯化铵。
实施例8
A、取硬脂酸74g,二乙醇胺2.4g,二乙烯三胺13g,于200℃反应5h,降温至120℃,得到反应料液,备用;
B、取水100g,聚二甲基二烯丙基氯化铵2g,混合、升温至50℃,得混合液,向混合液中加入步骤A所得反应料液12g,加入复合表面活性剂0.4g,滴加环氧氯丙烷10g,升温至70℃,保温反应2.3小时,加水5g,降温至室温,得到白色乳液,即为造纸施胶剂。
其中复合表面活性剂为质量比为3:2的烷基酚类聚氧乙烯醚和十六烷基三甲基氯化铵。
实施例9
A、取硬脂酸77g,二乙醇胺2.6g,二乙烯三胺14g,于210℃反应5h,降温至115℃,得到反应料液,备用;
B、取水100g,阳离子玉米淀粉10g,混合后,于90℃糊化1h,降温至50℃,得糊化淀粉液,向糊化淀粉液中加入步骤A所得反应料液13g,加入复合表面活性剂0.9g,滴加环氧氯丙烷6g,升温至70℃,保温反应2.7小时,加水4g,降温至室温,得到白色乳液,即为造纸施胶剂。
其中复合表面活性剂为质量比为1:1的OP-10和十六烷基三甲基氯化铵。
实施例10
A、取硬脂酸66g,二乙醇胺2.1g,二乙烯三胺10g,于200℃反应5h,降温至120℃,得到反应料液,备用;
B、取水100g,聚二甲基二烯丙基氯化铵7g,混合、升温至50℃,得混合液,向混合液中加入步骤A所得反应料液11g,加入复合表面活性剂0.5g,滴加环氧氯丙烷7g,升温至70℃,保温反应2.4小时,加水5g,降温至室温,得到白色乳液,即为造纸施胶剂。
其中复合表面活性剂为质量比为1:1的OP-12和十六烷基三甲基氯化铵。
二、施胶效果试验
1、对草浆抄纸施胶效果
(1)抄纸
取所需量的漂白麦草浆,加水浸泡后打浆,加入施胶剂,不加其他造纸助剂,按85g/m2定量抄片、压榨并烘干,纸张厚度0.207mm。
(2)检测
纸张施胶度按国家标准的液体渗透法测定;纸张柔软度按国家标准测定。检测结果如下。
表1
注:施胶剂用量为0.2%。
表2
项目 | 施胶度/s |
实施例1 | 17 |
实施例2 | 16 |
实施例3 | 16 |
实施例4 | 17 |
实施例5 | 17 |
实施例6 | 17 |
实施例7 | 16 |
实施例8 | 16 |
实施例9 | 16 |
实施例10 | 17 |
AKD乳液 | 12 |
阳离子双硬脂酸酰胺乳液 | 4 |
注:施胶剂用量为0.5%。
表3
项目 | 施胶度/s |
实施例1 | 23.5 |
实施例2 | 24 |
实施例3 | 23.5 |
实施例4 | 24 |
实施例5 | 24 |
实施例6 | 23 |
实施例7 | 23.5 |
实施例8 | 24 |
实施例9 | 23.5 |
实施例10 | 24 |
AKD乳液 | 18 |
阳离子双硬脂酸酰胺乳液 | 12.8 |
注:施胶剂用量为1.0%。
由表1-3可知,相同施胶量下,本发明的造纸施胶剂的施胶效果更好,施胶度相较于现有施胶剂高。
2、吸水度试验
将施胶剂施胶在纸张原纸上,施胶量为3.7g/m2,使其通过105℃的旋转式滚筒干燥机1min进行干燥,得到施胶纸。按照JISP-8140测定可勃值(g/m2),设定与水的接触时间为5分钟,数值越小表示施胶度越良好、抗水性能更好。
表4
项目 | 可勃吸水度(g/m2) |
实施例1 | 25 |
实施例2 | 22 |
实施例3 | 23 |
实施例4 | 24 |
实施例5 | 22 |
实施例6 | 23 |
实施例7 | 24 |
实施例8 | 25 |
实施例9 | 24 |
实施例10 | 23 |
AKD乳液 | 39 |
阳离子双硬脂酸酰胺乳液 | 68 |
由表4可知,本发明制备的造纸施胶剂抗水性更好。
3、产品稳定性试验
将得到的阳离子硬酯酰胺乳液在1h、24h、48h、64h进行粘度测定,结果本发明得到的阳离子硬酯酰胺乳液在64h后的粘度波动率小于20%,现有阳离子双硬脂酸酰胺乳液的粘度波动率大于70%。可见,本发明方法制备的造纸施胶剂稳定性更好。
4、施胶于瓦楞纸试验
将施胶剂用于瓦楞板时,考察瓦楞板的环压强度和耐破强度,防潮性能,控制施胶量均为5g/m2,在鼓风干燥箱中干燥10min,烘干后,将纸样进行恒温恒湿平衡处理,瓦楞纸进行环压强度和耐破度测试,并且把是施胶后的纸样放入到温度25度,湿度为90%的条件下放置2小时进行重新检测横向环压,结果如下:
表5
由表5可知,本发明施胶剂施胶后瓦楞纸的横向环压强度指数、纵向环压强度指数、耐破指数、防潮性能均优于现有技术,效果更好。
5、将施胶剂用于铜版纸时,考察铜版纸的抗张指数和耐折度,控制施胶量均为5g/m2,在鼓风干燥箱中干燥10min,烘干后,将纸样进行恒温恒湿平衡处理,铜版纸进行抗张指数和耐折度测试。结果如下:
表6
由表5可知,本发明施胶剂施胶后铜版纸的横向抗张指数、纵向抗张指数、横向耐折度、纵向耐折度均优于现有技术,效果更好。
6、纸样表面强度、平滑度、挺度测定试验
以静电复印纸作为施胶原纸,在施胶机上,以相同的施胶量(单面1.5g/m2)进行施胶,施胶后的纸样以相同的温度、时间(85℃*20s)在上光机上进行干燥,检测纸样表面强度、平滑度、挺度指标,结果如下。
表7
由表7可知,本发明的施胶剂施胶后静电复印纸的表面强度、平滑度和挺度效果均得到明显改善,且优于现有施胶剂施胶效果。
Claims (8)
1.一种新型造纸施胶剂的制备方法,其特征在于,包括以下步骤:
A、按重量份数计,取硬脂酸60-80份,二乙醇胺2-3份,二乙烯三胺6-14份,于140-220℃反应4-6h,降温至110-120℃,得到反应料液,备用;
B、按重量份数计,取水100份,淀粉2-10份,混合、糊化后,降温至45-50℃,得糊化淀粉液,或取水100份,高分子聚合物0.5-10份,混合、升温至50℃,得混合液;向糊化淀粉液或混合液中加入步骤A所得反应料液5-14份,加入复合表面活性剂0.2-1份,滴加环氧氯丙烷3-10份,升温至70-75℃,保温反应2-5小时,加水4-6份,降温至室温,得到白色乳液即为造纸施胶剂。
2.根据权利要求1所述的一种新型造纸施胶剂的制备方法,其特征在于,步骤B中的淀粉选自经过阳离子化或者氧化后的玉米淀粉或木薯淀粉。
3.根据权利要求1所述的一种新型造纸施胶剂的制备方法,其特征在于,将步骤B中的水和淀粉混合后,于90-95℃糊化45-60min。
4.根据权利要求1所述的一种新型造纸施胶剂的制备方法,其特征在于,步骤B中的高分子聚合物为具有1000至10万低分子分子量、阳电荷密度大的多胺型聚合物。
5.根据权利要求1所述的一种新型造纸施胶剂的制备方法,其特征在于,高分子聚合物选自聚酰胺环氧氯丙烷树脂、聚乙烯亚胺、阳离子聚丙烯酰胺、聚二甲基二烯丙基氯化铵中的一种或几种组合。
6.根据权利要求1所述的一种新型造纸施胶剂的制备方法,其特征在于,所述的复合表面活性剂包括非离子型表面活性剂和阳离子型表面活性剂。
7.根据权利要求6所述的一种新型造纸施胶剂的制备方法,其特征在于,非离子型表面活性剂选自聚氧乙烯醚类表面活性剂或聚氧乙烯脂肪酸酯,HLB值要求在10-15之间。
8.根据权利要求6所述的一种新型造纸施胶剂的制备方法,其特征在于,阳离子表面活性剂为具有碳链在10-18之间的、HLB值在15-17的烷基季胺盐类的阳离子表面活性剂。
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Application publication date: 20180629 |