CN107674629A - 一种单组分湿固化聚氨酯家具封边胶及其制备方法 - Google Patents
一种单组分湿固化聚氨酯家具封边胶及其制备方法 Download PDFInfo
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- CN107674629A CN107674629A CN201710599148.5A CN201710599148A CN107674629A CN 107674629 A CN107674629 A CN 107674629A CN 201710599148 A CN201710599148 A CN 201710599148A CN 107674629 A CN107674629 A CN 107674629A
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- Prior art keywords
- edge sealing
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- sealing glue
- solvent
- polyurethane
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Classifications
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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- C09J175/04—Polyurethanes
- C09J175/06—Polyurethanes from polyesters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08F220/20—Esters of polyhydric alcohols or phenols, e.g. 2-hydroxyethyl (meth)acrylate or glycerol mono-(meth)acrylate
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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- C08F220/24—Esters containing halogen containing perhaloalkyl radicals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F230/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal
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- C08F230/08—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal containing silicon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
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- C—CHEMISTRY; METALLURGY
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Abstract
本发明公开了一种单组分湿固化聚氨酯家具封边胶及其制备方法;以质量份数计,其原料组成为:20‑35份多元醇,15‑25份异氰酸酯,0.001‑0.01份催化剂,25‑50份溶剂,3‑6份的扩链剂和3‑625‑50以及1‑3份有机硅改性的含氟丙烯酸酯共聚物。该发明所得聚氨酯胶粘剂具有良好的胶接性,储存性,耐水性和抗老化性,并且室温下可固化,可根据基材调节胶膜表面能,适用于家具木材的封边处理。本发明单组分湿固化的聚氨酯家具封边胶的制备方法步骤简单,制备工艺条件要求低,易于工业化生产。
Description
技术领域
本发明涉及聚氨酯胶粘剂技术领域,具体涉及一种单组分湿固化聚氨酯家具封边胶及其制备方法。
背景技术
聚氨酯胶粘剂是一种分子链中含有极性很强、化学活泼性很高的氨基甲酸酯基团(-NHCOO-)或异氰酸酯基(-NCO)的胶粘剂。因为其中的异氰酸酯和氨基甲酸酯基团,所以能与含有活泼氢的材料,如泡沫塑料、木材、皮革、织物、纸张、陶瓷等多孔材料,以及金属、玻璃、橡胶、塑料等表面光洁的材料都有着优良的化学粘合力。聚氨酯与被粘合材料之间产生的氢键作用会使分子内聚力增强,从而使粘接更加牢固。聚氨酯胶粘剂因为具有良好的韧性、可调节性、极佳的耐低温性能和优良的稳定性,所以应用领域不断扩大,在国内外成为发展最快的胶粘剂。
单组分聚氨酯胶粘剂可以分为湿固化型,热熔型,压敏型等。常用的是湿固化性,分子链中的异氰酸酯基团暴露在空气中时,能够与空气中或者基材表面的活泼氢发生反应,生成脲键,从而固化。对于木制家具而言,将木材边缘与木材封条粘接在一起,因为两种基材的材质不同,硬度不同,所以对聚氨酯胶粘剂的要求也相对较高。现有技术中,木材所使用的最多的单组分聚氨酯胶粘剂是溶剂型聚氨酯胶粘剂和热熔型聚氨酯胶粘剂,热熔型聚氨酯胶粘剂使用时需要加热,且有粘板现象,溶剂型聚氨酯胶粘剂有稳定性差,储存时间短的缺点。如何得到易储存,粘度小,粘接强度好的聚氨酯胶粘剂是现在的研究方向。
公开号为CN 102140327A中国发明专利申请公开了一种可储存的植物油基聚氨酯木材胶粘剂,通过选取带羟基的聚酯型植物油基多元醇作为软缎,一种或两种二异氰酸酯作为硬段,用催化剂加快反应,溶剂稀释之后得到。该植物油基聚氨酯胶粘剂具有原料可再生、耐老化、无甲醛释放、初粘力好等优点。但因为所选取的植物油基聚氨酯链段分子量较小,所制得的胶粘剂交联度较小,剪切强度较低,只有1.93N/mm2,同时在合成过程中体系反应较快容易凝胶,所得木材胶的贮存时间只有45天,贮存不当很容易遇湿气固化,达不到工业生产的要求和使用要求,不能产业化。
发明内容
本发明的目的在于提供一种初粘力大、容易涂覆、固化快、粘度适中、储存期3个月,能够在不同表面能的基材上涂覆且耐化学稳定性好的单组分湿固化聚氨酯家具封边胶及其制备方法。
与现有技术(公开号为CN 102140327A中国专利)相比,本发明合成一种有机硅改性的含氟丙烯酸酯共聚物,使用少量有机硅改性的含氟丙烯酸酯共聚物改性聚氨酯,得到表面张力可调的适应各种木材表面的胶粘剂,可减少胶粘剂涂覆木材表面时的渗入,避免浪费,同时粘接强度和热稳定性以及耐候性也有所提高;硅氧烷的加入也调节了胶粘剂的表面张力,减少胶粘剂涂覆木材表面时的渗入,因此,可以相应的降低胶粘剂的粘度,得到耐储存的木材胶。有机硅改性的含氟丙烯酸酯共聚物的加入克服了现有技术粘度较小、储存性好的聚氨酯胶粘剂容易渗入到木材表面的气孔中,导致粘接强度下降的问题,也解决粘度较大的聚氨酯胶粘剂往往储存时间较短的问题。并且调节硅氧烷的用量和种类,可以得到不同表面张力的胶粘剂,能适应不同的基材表面。本发明的单组分湿固化聚氨酯家具封边胶的剪切强度可达2.96N/mm2,粘度较小容易涂覆,表干时间缩短至15min、储存期长达6个月,能够在不同表面能的基材上涂覆且耐热性好。
本发明目的通过如下技术方案实现:
一种单组分湿固化的聚氨酯家具封边胶,其原料组分及其质量份数为:
所述单组分湿固化聚氨酯家具封边胶的剪切强度为2.3-3N/mm2,表干时间为15-23min、储存期为3-6个月。
所述单组分湿固化的聚氨酯家具封边胶的制备方法,其按下述步骤依次进行:
1)将2-羟基乙基丙烯酸酯、甲基丙烯酸三氟乙酯、γ-(甲基丙烯酰氧)丙基三甲氧基硅烷以及BOP混合,升温至80~85℃反应2-3h,冷却后即制得有机硅改性含氟丙烯酸酯共聚物溶液;
2)将多元醇和抗氧化剂在真空条件下混合加热到110-115℃时脱水,保证多元醇中不含有水分;
3)在反应釜中加入脱水后的多元醇和二异氰酸酯,多元醇与二异氰酸酯的用量按异氰酸酯指数R1值(异氰酸酯基(-NCO)与羟基(-OH)的摩尔比)为15~10投料,反应温度 60~65℃,N2氛围下剧烈搅拌反应;
4)加入催化剂,将体系升温至80-95℃充分搅拌反应,加入有机硅改性的含氟丙烯酸酯共聚物;
5)降温至60-65℃,缓慢加入用溶剂稀释的二元醇扩链剂,并控制体系温度在70℃以下,且保持不变;滴加完之后,升温至75℃-80℃充分搅拌反应;
6)将经溶剂稀释的三元醇扩链剂加入反应体系中扩链,滴加时温度控制在70℃-75℃,滴加完后,升温至75℃-80℃充分搅拌反应;
7)降温至40-50℃,加入用溶剂稀释的增粘树脂,75℃-80℃充分搅拌反应;
8)降温至室温,加入稳定剂,过滤后得到成品,密封保存。
为进一步实现本发明目的,优选地,以质量份数计,步骤1)中,2-羟基乙基丙烯酸酯用量为20-40份,甲基丙烯酸三氟乙酯的用量为20-30份,γ-(甲基丙烯酰氧)丙基三甲氧基硅烷的用量为20-30份,BOP的用量为以上三种原料总质量的0.1%-0.5%。
优选地,所述步骤2)中的多元醇是聚醚二醇和聚酯二醇中的至少一种;所述抗氧化剂是2-(2’-羟基-3’,5’-二[1,1-二甲基苯基])-苯并三唑、双[β(3-叔丁基-5-甲基-4-羟基苯基)丙酸]三甘醇酯、双(N,N-二甲基肼碳酰-4-氨基苯基)甲烷中的一种或两种。
优选地,步骤3)中的二异氰酸酯主要是HDI、MDI、TDI、IPDI、它们的聚合物中的一种或两种。
优选地,步骤4)中的催化剂是二月桂酸二丁基锡、二乙酸二丁基锡、二乙酸二辛基锡、马来酸二丁基锡、苯酚锡(II)、辛酸亚锡、三乙烯二胺、三乙胺中的一种或两种。
优选地,步骤5)中的二元醇扩链剂为1,4-丁二醇、1,6-己二醇、乙二醇、丙二醇、一缩二乙二醇、季戊四醇中的一种或两种;所述溶剂为乙酸乙酯、乙酸丁酯、二氯甲烷、丙酮、甲苯、邻苯二甲酸二丁酯、N,N-二甲基甲酰胺或邻苯二甲酸二丁酯。
优选地,所述步骤6)中的三元醇扩链剂为三羟甲基乙烷、三羟甲基丙烷、甘油和三甘醇中的一种或两种。
优选地,所述步骤7)中的增粘树脂为环氧树脂、萜烯树脂、松香树脂、丙烯酸树脂,氯丁橡胶和石油树脂中的一种或多种;步骤8)中的稳定剂是亚磷酸苯二异葵酯、苯并三唑、三甘醇双-3-丁基-4-羟基-5-甲基苯基丙酸酯和N,N-二苯基对苯二胺的一种或两种。
优选地,步骤5)所述用溶剂稀释的二元醇扩链剂的溶剂与二元醇扩连接的质量比为 2-5:1;步骤6)所述经溶剂稀释的三元醇扩链剂中的溶剂与三元醇的质量比为10-12:1;步骤7)所述用溶剂稀释的增粘树脂中溶剂与增粘树脂的质量比为5-8:1。
步骤5)每隔一段时间测一次反应体系中NCO的百分含量,当反应中NCO的含量达到理论值时,进行下一步反应。
步骤6)按照R3值为1.5-2.0,将用溶剂稀释的三元醇扩链剂缓慢加入反应体系中扩链,滴加时控制温度在70℃-75℃,滴加完后,升温至75℃-80℃反应。每隔一段时间测一次反应体系中NCO的百分含量,当反应中NCO的含量达到理论值时,进行下一步反应。
步骤8)倒入铁罐密封保存。
步骤2)中,优选地,所述聚酯二醇2000和聚酯二醇3000的摩尔比为1:1-2。
述步骤3)中搅拌的转速范围为300~350rpm。
优选地,以质量份数计,所述催化剂的加入量0.005~0.01份。
优选地,以质量份数计,所述步骤2)中原料用量为多元醇为25-30份。
优选地,以质量份数计,所述步骤3)中原料用量异氰酸酯为25-30份。
优选地,以质量分数计,所述溶剂的加入量为40-50份。
优选地,步骤4)-7)中的充分搅拌的转速为250-350rpm。
含氟化合物的高表面活性、高耐热性、高化学稳定性具有其他材料不可比拟的优势。有机硅改性的聚合物从分子链结构来看,它既含有优异的介电性、柔韧性、耐水性以及生物相容性的有机硅链段,同时又具有良好的热稳定性,耐候性及耐磨性的高分子链。本发明合成一种有机硅改性的含氟丙烯酸酯共聚物,与聚氨酯聚合可以改变聚氨酯表面的疏水性,同时可以增强聚氨酯胶黏剂良好的热稳定性和耐候性。木材表面因材料不同会有一些气孔,在施胶过程中会有部分浸润至这些气孔中,表面残留的胶变少,粘接性能降低。利用有机硅改性的含氟丙烯酸酯共聚物改性,改变聚氨酯的疏水性,表面张力适当变大,气孔浸润量减少,不易造成浪费。同时,可以适当降低聚氨酯胶粘剂的粘度,制得更加稳定的木材胶。
与现有技术相比,本发明具有如下突出效果:
(1)本发明使用少量有机硅改性的含氟丙烯酸酯共聚物改性聚氨酯胶粘剂得到表面张力可调的适应各种木材表面的胶粘剂,可减少胶粘剂涂覆木材表面时的渗入,避免浪费,同时粘接强度也有所提高,并且调节合成有机硅改性的含氟丙烯酸酯共聚物的单体种类,可以的到不同表面张力的胶粘剂,能适应不同的基材表面。
(2)一般情况下,粘度越小的聚氨酯胶粘剂表现出越好的储存性能,但是对于木材胶,粘度较小的胶粘剂更容易渗入到木材表面的气孔中,导致粘接强度下降,而粘度较大的胶粘剂往往储存时间较短。本发明硅氧烷的加入调节了胶粘剂的表面张力,减少胶粘剂涂覆木材表面时的渗入,因此,可以相应的降低胶粘剂的粘度,得到耐储存的木材胶。
(3)本发明采用二吗啉二乙基醚作为催化剂效果较好,由于其在反应过程中不会催化异氰酸酯本身的自聚反应,只加快异氰酸酯基与醇羟基的反应,使得反应体系不会过度交联,避免凝胶;而且涂胶后可以加快异氰酸酯基与空气中的水分反应。因此,胶粘剂的固化时间变快,且不影响稳定性。而三乙烯二胺以及锡类催化剂只能催化异氰酸酯基同醇羟基的反应,涂胶后不能加快异氰酸酯基和水的反应,导致涂胶表面的固化速度慢,表干时间较长。
(4)加入高结晶度松香树脂和萜烯树脂以及氯丁橡胶等,提升了体系的固化速率,同时增加了木材胶各方面的力学性能,拉伸强度和剪切强度都有明显提升。
(5)引入少量二异氰酸酯三聚体,可以增大反应中体系的交联度,提高木材胶的粘结强度,缩短表干时间。
具体实施方式
为更好地理解本发明,下面结合实施例对本发明作进一步的说明,但本发明的实施方式不限如此。
实施例1(对比例)
一种单组分湿固化聚氨酯家具封边胶的制备方法,原料配方组成如下:
按照以上配比,将真空脱水后的聚酯二醇、2,4-甲苯二异氰酸酯、2-(2’-羟基-3’5’-二[1,1- 二甲基苯基])-苯并三唑抗氧化剂分别加入反应釜中,控制反应温度60~65℃,N2氛围下充分搅拌反应30min。随后,向反应釜中加入1.5g二月桂酸锡二丁基锡,体系升温至95℃反应3h。每隔半小时测一次NCO含量,当NCO含量达到18%-19%时,将体系降温至65℃,向其中恒速滴加80g 1,4-丁二醇,按质量比1:2用乙酸乙酯溶剂稀释,30min内滴完,升温至75℃反应1h,反应过程中分2次加入300g乙酸乙酯,每隔20min测一次NCO含量,当NCO的含量达到9%-11%时(理论设计的值时)降温至70℃,向其中加入40g三羟甲基丙烷(按质量比1:10,用乙酸乙酯稀释),控制反应温度为70℃不变,反应1h。反应完成后测体系的NCO含量达到5%-7%理论设计的值时,加入150g松香树脂(按质量比1:5比例用乙酸乙酯溶剂稀释),回流2h。将体系温度降至40℃,加入30g苯并三唑,搅拌30min 后出料。过筛后装入密封铁桶中。
实施例2
(1)有机硅改性的含氟丙烯酸酯共聚物的合成
将40g 2-羟基乙基丙烯酸酯和20g甲基丙烯酸三氟乙酯、20gγ-(甲基丙烯酰氧)丙基三甲氧基硅烷以及0.5g的BOP混合,升温至80~85℃反应3h,冷却后即制得有机硅改性含氟丙烯酸酯共聚物溶液。
(2)一种单组分湿固化聚氨酯家具封边胶的制备方法,原料配方组成如下:
按照以上配比,将真空脱水后的聚酯二醇、2,4-甲苯二异氰酸酯、2-(2’-羟基-3’5’-二[1,1- 二甲基苯基])-苯并三唑分别加入反应釜中,控制反应温度60~65℃,N2氛围下充分搅拌反应30min。随后,向反应釜中加入1.5g二月桂酸锡二丁基锡,体系升温至95℃反应3h。每隔半小时测一次NCO含量,当反应中NCO的含量达到50%时,加入30g有机硅改性的含氟丙烯酸酯共聚物继续反应。当NCO含量达到16%-17%时,将体系降温至65℃,向其中恒速滴加80g 1,4-丁二醇(按质量比1:2用乙酸乙酯稀释),30min内滴完,升温至75℃反应1h,每隔20min测一次NCO含量,当NCO的含量达到7%-9%时,降温至70℃,向其中加入30g三羟甲基丙烷(按质量比1:10比例用乙酸乙酯稀释),控制反应温度为70℃不变,反应1h,反应过程中分2次加入300g乙酸乙酯。反应完成后测体系的NCO含量达到 4%-5%时,加入150g松香树脂(按质量比1:5比例用乙酸乙酯稀释),回流2h。将体系温度降至40℃,加入30g苯并三唑,搅拌30min后出料。过筛后装入密封铁桶中。
实施例3
(1)有机硅改性的含氟丙烯酸酯共聚物的合成
将20g 2-羟基乙基丙烯酸酯和20g甲基丙烯酸三氟乙酯、20gγ-(甲基丙烯酰氧)丙基三甲氧基硅烷以及0.1g的BOP混合,升温至80~85℃反应2.5h,冷却后即制得有机硅改性含氟丙烯酸酯共聚物溶液。
(2)一种单组分湿固化聚氨酯家具封边胶的制备方法,原料配方组成如下:
按照以上配比,将真空脱水后的聚酯二醇、2,4-甲苯二异氰酸酯、双[β(3-叔丁基-5-甲基-4-羟基苯基)丙酸]三甘醇酯分别加入反应釜中,控制反应温度60~65℃,N2氛围下充分搅拌反应30min。随后,向反应釜中加入催化剂二吗啉二乙基醚,体系升温至95℃反应3.5h。每隔半小时测一次NCO含量,当反应中NCO的含量达到50%时,加入合成的有机硅改性的含氟丙烯酸酯共聚物,继续反应。当NCO含量达到16%-17%时,将体系降温至65℃,向其中恒速滴加80g 1,4-丁二醇(按质量比1:3用乙酸乙酯稀释),30min内滴完,升温至 75℃反应1h,每隔20min测一次NCO含量,当NCO的含量达到7%-9%时,降温至70℃,向其中加入30g三羟甲基丙烷(按质量比1:10比例用乙酸乙酯稀释),控制反应温度为70℃不变,反应1h,反应过程中分2次加入300g乙酸乙酯。反应完成后测体系的NCO含量达到4%-5%时,加入150g松香树脂(按质量比1:6比例用乙酸乙酯稀释),回流2h。将体系温度降至40℃,加入30g亚磷酸苯二异葵酯,搅拌30min后出料。过筛后装入密封铁桶中。
实施例4
(1)有机硅改性的含氟丙烯酸酯共聚物的合成
将30g 2-羟基乙基丙烯酸酯和20g甲基丙烯酸三氟乙酯、20gγ-(甲基丙烯酰氧)丙基三甲氧基硅烷以及0.3g的BOP混合,升温至80~85℃反应3h,冷却后即制得有机硅改性含氟丙烯酸酯共聚物溶液。
(2)一种单组分湿固化聚氨酯家具封边胶的制备方法,原料配方组成如下:
按照以上配比,将真空脱水后的聚酯二醇、2,4-甲苯二异氰酸酯、双(N,N-二甲基肼碳酰-4-氨基苯基)甲烷分别加入反应釜中,控制反应温度60~65℃,N2氛围下充分搅拌反应 30min。随后,向反应釜中加入三乙烯二胺,体系升温至95℃反应4h。每隔半小时测一次 NCO含量,当反应中NCO的含量达到70%时,加入甲苯二异氰酸酯三聚体,当反应中NCO的含量达到50%时,加入有机硅改性的含氟丙烯酸酯共聚物,继续反应。当NCO含量达到18%-20%时,将体系降温至65℃,向其中恒速滴加1,6-己二醇(按质量比1:4比例用甲苯稀释),30min内滴完,升温至75℃反应1h,每隔20min测一次NCO含量,当NCO的含量达到8%-10%时,降温至70℃,向其中加入三羟甲基丁烷(按质量比1:11比例用甲苯稀释),控制反应温度为70℃不变,反应1h,反应过程中分两次加入300g甲苯降低粘度。反应完成后测体系的NCO含量达到4%-6%时,加入萜烯树脂(按质量比1:8比例用甲苯稀释),回流2h。将体系温度降至40℃,加入N,N-二苯基对苯二胺,搅拌30min后出料,过筛后装入密封铁桶中。
实施例5
(1)有机硅改性的含氟丙烯酸酯共聚物的合成
将40g 2-羟基乙基丙烯酸酯和30g甲基丙烯酸三氟乙酯、20gγ-(甲基丙烯酰氧)丙基三甲氧基硅烷以及0.5g的BOP混合,升温至80~85℃反应3h,冷却后即制得有机硅改性含氟丙烯酸酯共聚物溶液。
(2)一种单组分湿固化聚氨酯家具封边胶的制备方法,原料配方组成如下:
按照以上配比,将真空脱水后的聚酯二醇、2,4-甲苯二异氰酸酯、双(N,N-二甲基肼碳酰-4-氨基苯基)甲烷分别加入反应釜中,控制反应温度60~65℃,N2氛围下充分搅拌反应 30min。随后,向反应釜中加入二吗啉二乙基醚,体系升温至95℃反应4h。每隔半小时测一次NCO含量,当反应中NCO的含量达到70%时,加入甲苯二异氰酸酯三聚体,当反应中NCO的含量达到50%时,加入有机硅改性的含氟丙烯酸酯共聚物,继续反应。当NCO 含量达到18%-20%时,将体系降温至65℃,向其中恒速滴加一缩二乙二醇(按质量比1:2 比例用甲苯稀释),30min内滴完,升温至75℃反应1h,每隔20min测一次NCO含量,当 NCO的含量达到9%-11%时,降温至70℃,向其中加入三羟甲基丙烷(按质量比1:12比例用甲苯稀释),控制反应温度为70℃不变,反应1h,反应过程中分两次加入甲苯200g降低体系粘度。反应完成后测体系的NCO含量达到5%-7%时,加入氯丁橡胶(按质量比1:8 比例用甲苯稀释),回流2h。将体系温度降至40℃,加入N,N-二苯基对苯二胺,搅拌30min 后出料。过筛后装入密封铁桶中。
以下是用于测试的木材胶膜的水接触角和吸水率、力学性能、耐热性能和粘接性能试验:
1)接触角测试
将所得木材胶倒入聚四氟乙烯模具中成膜,室温条件下放置3天,之后放入真空干燥箱中60℃干燥24h,确保胶膜中的溶剂完全去除。使用上海中晨JC2000C1型接触角测量仪测定聚氨酯胶膜的水接触角,测定温度25℃。所有样品的接触角的测量数据均重复5 次以获得可靠数值。吸水率测试将水性聚氨酯复合膜剪裁成10×10×2mm3规格,60℃干燥24小时至恒重后浸入去离子水中,37℃浸泡一段时间。吸水率可根据下式计算得到:
WA(%)=[(M1–M0)/M0]×100%
其中,M1是涂膜浸泡去离子水后的质量,M0是样品干燥时的质量。
所得结果如下表1所示:
表1
2)力学性能测试
对实施例1-5中样品进行力学性能分析,通过SMT-5000拉力试验机进行测试,按照GB/T528-1998的标准来评价样品的拉伸强度和断裂伸长率,以及HG/T3321-2012的标准来评价样品的弹性模量,所得结果如下表2所述:
表2
3)耐热性能测试
取固化的胶膜各9块,放入150℃的烘箱烘烤,分别在1h,3h,5h后取出,按照 GB/T528-1998的标准来评价样品的拉伸强度和断裂伸长率,检测耐热性能(测量3次取平均值)。
表3
4)粘接性能测试
剪一段跟木材边大小一致的封条,将所得聚氨酯木材胶均匀涂敷在木材和封条表面,室温下放置15-25分钟,直至表面固化,将涂胶两面贴合,按压紧实之后,室温下放置24h。破坏粘合层,定性分析其粘接性能。
将步骤1中处理好的样品固定在SMT-5000拉力试验机夹具上,做匀速拉伸,使粘合层承受越来越大的剪切力,直至粘合层分离。按照GB/T8165-2008的标准来评价样品的剪切强度,按照GB/T2794-1981的标准来评价样品的黏度。
表4
结果表明,在五组实施例中,实施例5表现出更好的机械性能、耐热性、粘接性能和贮存时间长的优点。对比实施例1(对比例),加入有机硅改性的含氟丙烯酸酯共聚物的实施例2-5表现更小的吸水率和更好的耐热性,因胶粘剂的粘度减小,贮存时间也相应延长。引入少量甲苯二异氰酸酯三聚体后,胶粘剂的表干时间缩短,放置24h后可破坏基材,粘接强度得到明显提升,得到一种性能优良的聚氨酯木材胶。本发明的单组分湿固化聚氨酯家具封边胶的剪切强度由1.94N/mm2提高至2.37-2.96N/mm2,粘度较小容易涂覆,表干时间由25min缩短至15-23min、储存期长达3-6个月,能够在不同表面能的基材上涂覆且耐热性好,相比于现有技术以及对比例,本发明单组分湿固化的聚氨酯家具封边胶在剪切强度、存储期有显著的改进,综合性能有明显的提升。
Claims (10)
1.一种单组分湿固化的聚氨酯家具封边胶,其特征在于其原料组分及其质量份数为:
所述单组分湿固化聚氨酯家具封边胶的剪切强度为2.3-3N/mm2,表干时间为15-23min、储存期为3-6个月。
2.权利要求1所述单组分湿固化的聚氨酯家具封边胶的制备方法,其特征在于其按下述步骤依次进行:
1)将2-羟基乙基丙烯酸酯、甲基丙烯酸三氟乙酯、γ-(甲基丙烯酰氧)丙基三甲氧基硅烷以及BOP混合,升温至80~85℃反应2-3h,冷却后即制得有机硅改性含氟丙烯酸酯共聚物溶液;
2)将多元醇和抗氧化剂在真空条件下混合加热到110-115℃时脱水,保证多元醇中不含有水分;
3)在反应釜中加入脱水后的多元醇和二异氰酸酯,多元醇与二异氰酸酯的用量按异氰酸酯基与羟基的摩尔比为15~10投料,反应温度60~65℃,N2氛围下搅拌反应;
4)加入催化剂,将体系升温至80-95℃充分搅拌反应,加入有机硅改性的含氟丙烯酸酯共聚物;
5)降温至60-65℃,缓慢加入用溶剂稀释的二元醇扩链剂,并控制体系温度在70℃以下,且保持不变;滴加完之后,升温至75℃-80℃充分搅拌反应;
6)将经溶剂稀释的三元醇扩链剂加入反应体系中扩链,滴加时温度控制在70℃-75℃,滴加完后,升温至75℃-80℃充分搅拌反应;
7)降温至40-50℃,加入用溶剂稀释的增粘树脂,75℃-80℃充分搅拌反应;
8)降温至室温,加入稳定剂,过滤后得到成品,倒入铁罐密封保存。
3.根据权利要求2所述的单组分湿固化的聚氨酯家具封边胶的制备方法,其特征在于,以质量份数计,步骤1)中,2-羟基乙基丙烯酸酯用量为20-40份,甲基丙烯酸三氟乙酯的用量为20-30份,γ-(甲基丙烯酰氧)丙基三甲氧基硅烷的用量为20-30份,BOP的用量为以上三种原料总质量的0.1%-0.5%。
4.根据权利要求2所述的单组分湿固化的聚氨酯家具封边胶的制备方法,其特征在于,所述步骤(2)中的多元醇是聚醚二醇和聚酯二醇中的至少一种;所述抗氧化剂是2-(2’-羟基-3’,5’-二[1,1-二甲基苯基])-苯并三唑、双[β(3-叔丁基-5-甲基-4-羟基苯基)丙酸]三甘醇酯、双(N,N-二甲基肼碳酰-4-氨基苯基)甲烷中的一种或两种。
5.根据权利要求2所述的单组分湿固化的聚氨酯家具封边胶的制备方法,其特征在于,步骤(3)中的二异氰酸酯主要是HDI、MDI、TDI、IPDI、它们的聚合物中的一种或两种。
6.根据权利要求2所述的单组分湿固化的聚氨酯家具封边胶的制备方法,其特征在于,步骤(4)中的催化剂是二月桂酸二丁基锡、二乙酸二丁基锡、二乙酸二辛基锡、马来酸二丁基锡、苯酚锡(II)、辛酸亚锡、三乙烯二胺、三乙胺中的一种或两种。
7.根据权利要求2所述的单组分湿固化的聚氨酯家具封边胶的制备方法,其特征在于,步骤(5)中的二元醇扩链剂为1,4-丁二醇、1,6-己二醇、乙二醇、丙二醇、一缩二乙二醇、季戊四醇中的一种或两种;所述溶剂为乙酸乙酯、乙酸丁酯、二氯甲烷、丙酮、甲苯、邻苯二甲酸二丁酯、N,N-二甲基甲酰胺或邻苯二甲酸二丁酯。
8.根据权利要求2所述的单组分湿固化的聚氨酯家具封边胶的制备方法,其特征在于,所述步骤(6)中的三元醇扩链剂为三羟甲基乙烷、三羟甲基丙烷、甘油和三甘醇中的一种或两种。
9.根据权利要求2所述的单组分湿固化的聚氨酯家具封边胶的制备方法,其特征在于,所述步骤(7)中的增粘树脂为环氧树脂、萜烯树脂、松香树脂、丙烯酸树脂,氯丁橡胶和石油树脂中的一种或多种;步骤(8)中的稳定剂是亚磷酸苯二异葵酯、苯并三唑、三甘醇双-3-丁基-4-羟基-5-甲基苯基丙酸酯和N,N-二苯基对苯二胺的一种或两种。
10.根据权利要求2所述的单组分湿固化的聚氨酯家具封边胶的制备方法,其特征在于,步骤5)所述用溶剂稀释的二元醇扩链剂的溶剂与二元醇扩连接的质量比为2-5:1;步骤6)所述经溶剂稀释的三元醇扩链剂中的溶剂与三元醇的质量比为10-12:1;步骤7)所述用溶剂稀释的增粘树脂中溶剂与增粘树脂的质量比为5-8:1。
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