CN106281182B - 人造板用水性聚氨酯无醛胶 - Google Patents
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Abstract
本发明公开了一种人造板用水性聚氨酯无醛胶,它由以下按重量份配比的原料混合制成:氧化纤维素组合物主胶75~95份、交联剂5~25份;所述氧化纤维素组合物主胶是由下述重量份的原料配制成:粒径为75~90μm的纤维粉200~265份、TEMPO 0.8~1.5份、溴化钠1.6~3.0份、活性氯含量为7.0~7.5%wt的次氯酸钠1.0~3.0份、PVA 30~50份、淀粉0~30份、尿素45~60份、NP‑10 3~3.5份、亚硫酸氢钠15~18份和水650~1000份;所述交联剂是由下述按重量份原料制成:表面活性剂AEO或/和OS 10份、液体聚MDI 84~113份。本发明无醛胶适用期合适,可满足现有的人造板生产工艺要求,且粘合强度高、耐水性好,生产成本相对较低。
Description
技术领域
本发明属胶粘剂技术领域,具体是一种人造板用水性聚氨酯无醛胶。
背景技术
采用水性聚氨酯取代三醛胶粘剂,以避免甲醛对人体健康的危害,应用于中纤板、刨花板、胶合板等木质人造板生产已多有报道。应用于木材粘合的水性聚氨酯技术,有直接将聚氨酯分散于水作为胶粘剂,或利用乙烯基单体聚合乳液为主胶、异氰酸酯为固化剂形成胶粘剂等。如中国专利申请公开号CN 103347917 A公开的一种基于聚异氰酸酯的水性胶粘剂,它包含有机聚异氰酸酯、异氰酸酯-反应性化合物和促进异氰酸酯-三聚的催化剂。如美国专利US 4944823公开的利用二苯甲烷-4,4'-二异氰酸酯与淀粉或糖混合物,或反应形成的糖类聚氨酯,加水混合均匀后可用于制造颗粒板和胶合板。如中国专利申请公开号CN1285695 C提出的一种聚合多异氰酸酯交联水性乙烯基乳液粘合剂,它采用水、聚乙烯醇、乙酰化聚乙烯醇、醋酸乙烯酯、丙烯酸丁酯、甲基丙烯酸、复合乳化剂、过硫酸铵、滑石粉、羧基丁苯乳胶合成乳液,以水乳化多异氰酸酯和高官能度多异氰酸酯混合物作为交联剂。如中国专利申请公开号CN 104962218 A中公开的一种胶合板用异氰酸酯改性VAE乳液无醛胶黏剂,它包含以下组分原料:VAE乳液、松香酯乳液、异氰酸酯、轻质碳酸钙。如中国专利申请分开号CN 101503609 B中公开的一种非甲醛类水性高分子复合胶粘剂的制备方法,它方法包括:1、将十七烷基聚氧乙烯醚、聚氧化丙烯二醇等多元醇与多异氰酸酯单体的二聚体、三聚体或多聚体反应得预聚体;2、将脂肪醇聚氧化乙烯醚、烷基酚聚氧化乙烯醚等乳化剂与果胶酸盐、酪朊酸盐等稳定剂加入水中,搅拌得混合溶液;2、将预聚体加入到混合溶液中搅拌得到异氰酸酯乳液;4、将异氰酸酯乳液与水性高分子混合得水性高分子复合胶粘剂。
上述技术应用于人造板生产,取得无醛、粘合强度高、耐水性好的粘合效果。但是存在生产成本过高、胶粘剂适用期短、不大适应现有的人造板生产工艺要求等缺点。
发明内容
本发明所要解决的技术问题是提供一种人造板用水性聚氨酯无醛胶,该无醛胶的粘合强度高、耐水性好,且成本相对较低,能满足现有的人造板生产工艺要求。
本发明以如下技术方案解决上述技术问题:
本发明人造板用水性聚氨酯无醛胶,它由以下按重量份配比的原料混合制成:氧化纤维素组合物主胶75~95份、交联剂5~25份;
所述氧化纤维素组合物主胶的制备方法是:
原料按重量份配比是:粒径为75~90μm的纤维粉200~265份、TEMPO(2,2,6,6-四甲基哌啶-1-氧基自由基)0.8~1.5份、溴化钠1.6~3.0份、活性氯含量为7.0~7.5%wt的次氯酸钠1.0~3.0份、PVA(聚乙烯醇)30~50份、淀粉0~30份、尿素45~60份、NP-10(壬基酚聚氧乙烯醚)3~3.5份、亚硫酸氢钠15~18份和水650~1000份;
制备工艺是:在反应器中先放入水,然后加入纤维粉、TEMPO、溴化钠和次氯酸钠,在10~35℃下搅拌均匀并调整物料的pH值=9~11,反应1.5~2.0hr后升温至50℃,再加入PVA、淀粉和尿素,升温至90℃保温40~60min,测定涂-4杯粘度为10~25s后调整pH值=6.0,降温至45℃后再加入NP-10和亚硫酸氢钠,搅拌至溶解完全,出料备用;
所述交联剂的制备方法是:
所需原料按重量份配比是:表面活性剂AEO或/和OS(脂肪醇聚氧乙烯醚)10份、液体聚MDI(二苯基甲烷二异氰酸酯)84~113份;
制备工艺是:往干净、干燥的反应器内通氮气驱尽空气,在氮气保护下加入经脱水后的表面活性剂和聚MDI,常温搅拌30分钟,然后以1.5~2℃/min的升温速度升温至75℃,保温2h使物料澄清透明,再降温至40℃出料,得异氰酸酯封端预聚体,装入密闭的容器中贮存备用。
所述纤维粉为纸浆粉、微晶纤维素粉、木薯渣纤维粉、棉花纤维粉中的一种或一种以上混合。
所述PVA的聚合度为500~2400、醇解度为88~99%。
所述表面活性剂的EO平均摩尔数为9~15。
所述聚MDI的NCO含量为30~32.5%wt。
本发明产品水性聚氨酯无醛胶应用于人造板生产时,主胶和交联剂在施胶前混合均匀。用于纤维板制造时,施胶量为绝干纤维的16~20%wt,施胶干燥后的纤维含水率为10~12%wt。用于制造胶合板时,单板双面施胶量为200~350g/m2,单板含水率范围为12~35%wt,最适宜含水率为15~28%wt之间。用于刨花板制造时,施胶量为绝干刨花的8~10%wt(表、芯层同),施胶后刨花含水率:表层8~10%wt,芯层6~8%wt。
本发明在制备氧化纤维素组合物主胶的物料中的纤维素、木质素、PVA、淀粉均为多羟基化合物,在人造板热压过程中可与MDI形成纤维素-氨基甲酸酯、PVA-氨基甲酸酯和淀粉-氨基甲酸酯等聚氨酯结构。采用TEMPO/NaBr/NaClO循环的氧化体系,将纤维粉中的纤维素/木质素中大量的伯羟基氧化成醛基等活性基团。由于TEMPO的空间位阻效应,伯羟基的氧化速率远远大于仲羟基,使得反应有很高的选择性。醛基与脲形成纤维素/木质素脲醛衍生物,与其它组分一起形成复合胶粘体系。
本发明的交联剂在合成时,AEO/OS分子链中的一元醇与异氰酸酯反应,通过氨基甲酸酯基与聚氧乙烯重复单元连接在一起。所用的AEO/OS分子中具有足够长的聚氧乙烯重复单元链,使多异氰酸酯拥有较强的亲水能力;此外,聚氧乙烯分子链产生卷曲,将高活性的异氰酸酯保护起来,使其与氧化纤维素组合物主胶混合后获得稳定的均相乳液混合物。经测定,乳液混合物放置120min后NCO仍有80%左右未反应,因此,本发明胶粘剂亦在人造板热压时表现出良好的粘合性能。
本发明人造板用水性聚氨酯无醛胶可直接使用于现有(使用脲醛树脂胶的)人造板设备,即可生产NAF(使用不添加甲醛的胶粘剂)人造板,该无醛胶适用期合适,可满足现有的人造板生产工艺要求,且粘合强度高、耐水性好,生产成本相对较低。
具体实施方式
实施例1,制备氧化纤维素组合物主胶:
在反应器中先放入6800g的水,再加入2000g粒径为75μm的纸浆粉、12g的TEMPO、18g溴化钠和10g活性氯含量为7.5wt%的次氯酸钠,在35℃下搅拌均匀并用20%wt的氢氧化钠溶液调整物料的pH值=10,反应1.5hr后升温至50℃,再加入300g聚合度为2400、醇解度为88%的PVA以及300g玉米淀粉(预先用适量水调成浆状)和450g尿素,升温至90℃保温60min,测定涂-4杯粘度为25s,再用1∶4(V/V)的盐酸水溶液调整pH值=6.0,降温至45℃后再加入30g NP-10和150g亚硫酸氢钠,搅拌至溶解完全,出料备用。
实施例2,制备氧化纤维素组合物主胶:
在反应器中先放入1000g的水,再加入230g粒径80μm的木薯渣纤维粉、1.2g的TEMPO、2.5g溴化钠和3g活性氯含量为7.0wt%的次氯酸钠,在10℃下搅拌均匀并用20%wt的氢氧化钠溶液调整物料的pH值=11,反应2.0hr后升温至50℃,再加入46g聚合度为2400、醇解度为99%的PVA以及15.5g的木薯淀粉(预先用适量水调成浆状)和46g尿素,升温至90℃保温47min,测定涂-4杯粘度为20s,用1∶4(V/V)的盐酸水溶液调整pH值=6.0,降温至45℃后再加入3g的NP-10和15g亚硫酸氢钠,搅拌至溶解完全,出料备用。
实施例3,制备氧化纤维素组合物主胶:
在反应器中先放入1000g的水,再加入115g粒径为90μm的微晶纤维素粉和150g粒径为90μm的棉花纤维粉、1.5g的TEMPO、2.9g溴化钠和2.9g活性氯含量为7.2wt%的次氯酸钠,在27℃下搅拌均匀并用20%wt的氢氧化钠溶液调整物料的pH值=9,反应100min后升温至50℃,再加入29g聚合度为500、醇解度为88%的PVA和15g聚合度为1700、醇解度为99%的PVA和59g尿素,升温至90℃保温40min,测定涂-4杯粘度为18s,用1∶4(V/V)的盐酸水溶液调整pH值=6.0,降温至45℃后再加入3.5g的NP-10和18g亚硫酸氢钠,搅拌至溶解完全,出料备用。
实施例4
制备交联剂:往干净、干燥的反应器内通氮气驱尽空气,在氮气保护下加入经脱水后的100g的OS-15(EO摩尔数15、羟值57.80mgKOH/g)和840g的MDI(德国BASF M-20S,NCO含量30.80%),常温搅拌30分钟,然后以2℃/min的升温速度升温至75℃,保温2h物料澄清透明,降温至40℃出料,得异氰酸酯封端预聚体,装入密闭的容器中贮存备用。预聚体粘度为250mPa·s,NCO%含量为26.98%。
实施例5
制备交联剂:往干净、干燥的反应器内通氮气驱尽空气,在氮气保护下加入经脱水后的100g的AEO-9(EO摩尔数9、羟值96.05mgKOH/g)和1130g的MDI(中国万华PM200,NCO含量31.85%),常温搅拌30分钟,然后以1.5℃/min的升温速度升温至75℃,保温2h物料澄清透明,降温至40℃出料,得异氰酸酯封端预聚体,装入密闭的容器中贮存备用。预聚体粘度为265mPa·s,NCO%含量为27.46%。
实施例6
制备交联剂:往干净、干燥的反应器内通氮气驱尽空气,在氮气保护下加入经脱水后的50g的AEO-9(EO摩尔数9、羟值96.05mgKOH/g)和50g的OS-15(EO摩尔数15、羟值57.80mgKOH/g)以及1027g的MDI(日本NPU MR200,NCO含量30.85%),常温搅拌30分钟,然后以2℃/min的升温速度升温至75℃,保温2h物料澄清透明,降温至40℃出料,得异氰酸酯封端预聚体,装入密闭的容器中贮存备用。预聚体粘度为258mPa·s,NCO%含量为27.22%。
实施例7
按表1,采用实施例1~3的主胶和实施例4~6的交联剂配制本发明人造板用水性聚氨酯无醛胶,在施胶前将主胶和交联剂混合均匀。
按表1制作600×600mm人造板。其中胶合板:热压温度110℃,压力1.5MPa,时间840s;刨花板:热压温度180℃,压力2.0MPa,时间250s;中纤板:热压温度180℃,压力3.5MPa,时间300s。结果见表1:
表1
*1含水率:胶合板为未施胶前单板含水率;刨花板为施胶后刨花含水率;中纤板为施胶干燥后的纤维含水率。
*2施胶量:胶合板为单板双面施胶量;刨花板、中纤板为占绝干刨花/纤维的比例。
*3强度:胶合板为平均胶合强度(Ⅱ类板);刨花板、中纤板为内结合强度。
*4耐水性:胶合板为100×100mm试样沸水煮;刨花板为2hr厚度吸水膨胀率;中纤板为24hr厚度吸水膨胀率。
Claims (5)
1.人造板用水性聚氨酯无醛胶,其特征在于,它由以下按重量份配比的原料混合制成:氧化纤维素组合物主胶75~95份、交联剂5~25份;
所述氧化纤维素组合物主胶的制备方法是:
原料按重量份配比是:粒径为75~90μm的纤维粉200~265份、TEMPO 0.8~1.5份、溴化钠1.6~3.0份、活性氯含量为7.0~7.5%wt的次氯酸钠1.0~3.0份、PVA 30~50份、淀粉0~30份、尿素45~60份、NP-10 3~3.5份、亚硫酸氢钠15~18份和水650~1000份;
制备工艺是:在反应器中先放入水,然后加入纤维粉、TEMPO、溴化钠和次氯酸钠,在10~35℃下搅拌均匀并调整物料的pH值9~11,反应1.5~2.0hr后升温至50℃,再加入PVA、淀粉和尿素,升温至90℃保温40~60min,测定涂-4杯粘度为10~25s后调整pH值6.0,降温至45℃后再加入NP-10和亚硫酸氢钠,搅拌至溶解完全,出料备用;
所述交联剂的制备方法是:
原料按重量份配比是:表面活性剂AEO或/和OS 10份、液体聚MDI(二苯基甲烷二异氰酸酯)84~113份;
制备工艺是:往干净、干燥的反应器内通氮气驱尽空气,在氮气保护下加入经脱水后的表面活性剂和聚MDI,常温搅拌30分钟,然后以1.5~2℃/min的升温速度升温至75℃,保温2h使物料澄清透明,再降温至40℃出料,得异氰酸酯封端预聚体,装入密闭的容器中贮存备用。
2.根据权利要求1所述人造板用水性聚氨酯无醛胶,其特征在于,所述纤维粉为纸浆粉、微晶纤维素粉、木薯渣纤维粉、棉花纤维粉中的一种或一种以上混合。
3.根据权利要求1所述人造板用水性聚氨酯无醛胶,其特征在于,所述PVA的聚合度为500~2400、醇解度为88~99%。
4.根据权利要求1所述人造板用水性聚氨酯无醛胶,其特征在于,所述表面活性剂的EO平均摩尔数为9~15。
5.根据权利要求1所述人造板用水性聚氨酯无醛胶,其特征在于,所述聚MDI的NCO含量为30~32.5%wt。
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