CN104961376B - 一种聚羧酸高性能减水剂及其制备方法 - Google Patents
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Abstract
本发明公开了一种聚羧酸高性能减水剂及其制备方法,所述减水剂主要由甲基烯丙基聚氧乙烯醚,丙烯酸,巯基乙酸,抗坏血酸,双氧水,氢氧化钠,顺丁烯二酸酐,亚磷酸钠及纯化水制备而成。所述聚羧酸减水剂减水率高达45%,能较好的满足混凝土高减水和高保坍要求,对温度不敏感,水泥适应性强,且制备工艺简单,容易制得。
Description
技术领域
本发明涉及一种聚羧酸减水剂及其制备方法,特别是一种聚羧酸高性能减水剂及其制备方法。
背景技术
聚羧酸系高性能减水剂(液体)是继木钙为代表的普通减水剂和以萘系为代表的高效减水剂之后发展起来的第三代高性能减水剂,是目前世界上最前沿、科技含量最高、应用前景最好、综合性能最优的一种高效减水剂。PC聚羧酸系高性能减水剂是代表当今世界技术含量最领先的减水剂产品。经与国内外同类产品性能比较表明,PC聚羧酸系高性能减水剂在技术性能指标、性价比方面都达到了当今国际先进水平。
但是现有聚羧酸系减水剂的减水率通常是35%-40%,不能较好的满足混凝土减水和保坍要求,对温度敏感,且水泥适应性不强。
发明内容
本发明的目的在于,提供一种聚羧酸高性能减水剂及其制备方法。所述聚羧酸减水剂减水率高,流动性能好,能较好的满足混凝土高减水和高保坍要求,对温度不敏感,水泥适应性强,且制备工艺简单,容易制得。
为解决上述技术问题,本发明采用以下技术方案实现:一种聚羧酸高性能减水剂,按重量份计算,主要由甲基烯丙基聚氧乙烯醚25-50份,丙烯酸1-10份,巯基乙酸5-15份,抗坏血酸1-5份,双氧水10-15份,氢氧化钠10-20份,顺丁烯二酸酐1-10份,亚磷酸钠1-10份及纯化水制备而成。
前述的聚羧酸高性能减水剂中,按重量份计算,主要由甲基烯丙基聚氧乙烯醚30-40份,丙烯酸3-8份,巯基乙酸10-13份,抗坏血酸2-3份,双氧水12-13份,氢氧化钠13-17份,顺丁烯二酸酐3-8份,亚磷酸钠3-8份及纯化水制备而成。
前述的聚羧酸高性能减水剂中,按重量份计算,主要由甲基烯丙基聚氧乙烯醚35份,丙烯酸6份,巯基乙酸12份,抗坏血酸2.5份,双氧水2.5份,氢氧化钠15份,顺丁烯二酸酐5份,亚磷酸钠5份及纯化水制备而成。
一种如前述的聚羧酸高性能减水剂的制备方法,按下述步骤制备:
1、将甲基烯丙基聚氧乙烯醚用纯化水配制成浓度为20-25%的溶液,得A品;
2、将A品加入反应釜中,加热,直至反应釜内的温度升至60℃,得B品;
3、取滴加罐Ⅰ,依次向滴加罐Ⅰ加入丙烯酸、巯基乙酸、抗坏血酸、顺丁烯二酸酐和亚磷酸钠再向滴加罐Ⅰ加纯化水,使溶液浓度为25-30%,得C品;
4、取滴加罐Ⅱ,向滴加罐Ⅱ中加入双氧水,再向滴加罐Ⅱ中加纯化水,使溶液浓度为25-30%,得D品;
5、控制装B品的反应釜内的温度为58-62℃,依次向B品中滴加C品和D品;C品滴加时间2h,D品滴加时间2.5h,滴加完毕后,向反应釜中加入氢氧化钠,调节PH值为5-7;加入完毕后,保温2-3h后,将温度降至40-45℃,即得。
本发明所述聚羧酸减水剂主要由甲基烯丙基聚氧乙烯醚,丙烯酸,巯基乙酸,抗坏血酸,双氧水,氢氧化钠,顺丁烯二酸酐,亚磷酸钠及纯化水制备而成。其中丙烯酸,Acrylicacid,是重要的有机合成原料及合成树脂单体,是聚合速度非常快的乙烯类单体。是最简单的不饱和羧酸,由一个乙烯基和一个羧基组成。纯的丙烯酸是无色澄清液体,带有特征的刺激性气味。它可与水、醇、醚和氯仿互溶,是由从炼油厂得到的丙烯制备的。大多数用以制造丙烯酸甲酯、乙酯、丁酯、羟乙酯等丙烯酸酯类。丙烯酸及丙烯酸酯可以均聚及共聚,其聚合物用于合成树脂、合成纤维、高吸水性树脂、建材、涂料等工业部门。巯基乙酸,Mercaptoacetic acid,(化学式:C2H4O2S,式量:92.12)含硫有机化合物,无色透明液体,有强烈刺激性气味。熔点-16.5,沸点220℃,密度1.33g/mL。闪点>110℃,折射率1.5030。与水混溶,可混溶于乙醇、***,溶于普通溶剂。用于制作环氧树脂,双酚A的催化剂,是日用化妆品冷烫精及脱毛剂的主要原料。用于制作环氧树脂,双酚A的催化剂,是日用化妆品冷烫精及脱毛剂的主要原料,也可用作合成PVC透明塑料和有机锑,有机锡的热稳定剂的基础原料。其试剂产品是检验铁,钼,银,锡等金属离子的灵敏试剂。选矿上为硫化铜及硫化铁矿物的抑制剂。在石油化学工业和铁路部门,用于设备及铁轨的清洗除锈。抗坏血酸,又名维生素C,Ascorbic Acid,是高等灵长类动物与其他少数生物的必需营养素。抗坏血酸在大多的生物体可借由新陈代谢制造出来,但是人类是最显著的例外。最广为人知的是缺乏维生素C会造成坏血病。在生物体内,维生素C是一种抗氧化剂,保护身体免于自由基的威胁,维生素C同时也是一种辅酶。其广泛的食物来源为各类新鲜蔬果。双氧水,Hydrogen Peroxide,纯过氧化氢是淡蓝色的黏稠液体,可任意比例与水混合,是一种强氧化剂,水溶液俗称双氧水,为无色透明液体。其水溶液适用于医用伤口消毒及环境消毒和食品消毒。在一般情况下会分解成水和氧气,但分解速度极其慢,加快其反应速度的办法是加入催化剂——二氧化锰或用短波射线照射。双氧水的用途分医用、军用和工业用三种,日常消毒的是医用双氧水,医用双氧水可杀灭肠道致病菌、化脓性球菌,致病酵母菌,一般用于物体表面消毒。化学工业用作生产过硼酸钠、过碳酸钠、过氧乙酸、亚氯酸钠、过氧化硫脲等的原料,酒石酸、维生素等的氧化剂。医药工业用作杀菌剂、消毒剂,以及生产福美双杀虫剂和40l抗菌剂的氧化剂。印染工业用作棉织物的漂白剂,还原染料染色后的发色。用于生产金属盐类或其他化合物时除去铁及其他重金属。也用于电镀液,可除去无机杂质,提高镀件质量。还用于羊毛、生丝、象牙、纸浆、脂肪等的漂白。高浓度的过氧化氢可用作火箭动力助燃剂。氢氧化钠,Sodium hydroxide,,化学式为NaOH,俗称烧碱、火碱、苛性钠,为一种具有很强腐蚀性的强碱,一般为片状或颗粒形态,易溶于水(溶于水时放热)并形成碱性溶液,另有潮解性,易吸取空气中的水蒸气。NaOH是化学实验室其中一种必备的化学品,亦为常见的化工品之一。氢氧化铝为一相当常用于除去水中杂质的胶状凝聚剂,因过渡金属的氢氧化物大都不太溶于水,且氢氧化铝表面的面积大可以吸附小微粒,故于自来水中添加明矾可促使过渡金属以氢氧化物的形式沉淀析出,再利用简单的过滤设备,即可完成自来水的初步过滤。顺丁烯二酸酐,cis-butenedioic anhydride,。无色结晶,有强烈刺激气味,凝固点52.8℃,沸点202℃,易升华。主要由苯或碳四馏分中的正丁烷或丁烯氧化而制得,是生产不饱和聚酯及有机合成的原料。溶于乙醇、***等多种有机溶剂,难溶于石油醚和四氯化碳。与热水作用生成顺丁烯二酸。易于烯类单体进行共聚反应;也可进行均聚。与二元醇反应生成线型不饱和聚酯,与三氧化硫反应生成磺化顺丁烯二酸酐。塑料工业用于制造增塑剂。造纸工业用于制造纸张处理剂。合成树脂工业用于制造不饱和聚酯树脂、醇酸树脂等。涂料工业用于制造绝缘漆、白磁漆、烘漆、清漆等。农药工业用于制造农药马拉松和高效低毒农药4049等。医药工业用于制造长效磺胺药。油脂工业用作脂肪、油的防腐剂。有机工业用于制造富马酸及四氢呋喃等。分析化学中用作化学试剂。亚磷酸钠,Sodium phosphite,化学式:Na2HPO3·5H2O,白色结晶性粉末。易吸湿,易溶于水。其水溶液稳定。
与现有技术相比,本发明采用以上原料制成聚羧酸减水剂,各组分具有很好的协同作用,所制备的聚羧酸减水剂减水率高达45%,流动性能好,2h坍落度保留值大于180mm,能较好的满足混凝土高减水和高保坍要求,对温度不敏感,水泥适应性强,且制备工艺简单,容易制得。达到了发明目的。
下面结合实施例对发明作进一步的说明,但并不作为对本发明限制的依据。
具体实施方式:
实施例1.
配方:甲基烯丙基聚氧乙烯醚35g,丙烯酸6g,巯基乙酸12g,抗坏血酸2.5g,双氧水2.5g,氢氧化钠15g,顺丁烯二酸酐5g,亚磷酸钠5g及纯化水。
工艺:
1、将甲基烯丙基聚氧乙烯醚用纯化水配制成浓度为22%的溶液,得A品;
2、将A品加入反应釜中,加热,直至反应釜内的温度升至60℃,得B品;
3、取滴加罐Ⅰ,依次向滴加罐Ⅰ加入丙烯酸、巯基乙酸、抗坏血酸、顺丁烯二酸酐和亚磷酸钠再向滴加罐Ⅰ加纯化水,使溶液浓度为27%,得C品;
4、取滴加罐Ⅱ,向滴加罐Ⅱ中加入双氧水,再向滴加罐Ⅱ中加纯化水,使溶液浓度为27%,得D品;
5、控制装B品的反应釜内的温度为58-62℃,依次向B品中滴加C品和D品;C品滴加时间2h,D品滴加时间2.5h,滴加完毕后,向反应釜中加入氢氧化钠,调节PH值为5.5-6;加入完毕后,保温2-3h后,将温度降至40-45℃,即得减水剂。
实施例2.
配方:甲基烯丙基聚氧乙烯醚40g,丙烯酸8g,巯基乙酸13g,抗坏血酸3g,双氧水13g,氢氧化钠17g,顺丁烯二酸酐8g,亚磷酸钠8g及纯化水。
工艺:
1、将甲基烯丙基聚氧乙烯醚用纯化水配制成浓度为25%的溶液,得A品;
2、将A品加入反应釜中,加热,直至反应釜内的温度升至60℃,得B品;
3、取滴加罐Ⅰ,依次向滴加罐Ⅰ加入丙烯酸、巯基乙酸、抗坏血酸、顺丁烯二酸酐和亚磷酸钠再向滴加罐Ⅰ加纯化水,使溶液浓度为30%,得C品;
4、取滴加罐Ⅱ,向滴加罐Ⅱ中加入双氧水,再向滴加罐Ⅱ中加纯化水,使溶液浓度为30%,得D品;
5、控制装B品的反应釜内的温度为58-62℃,依次向B品中滴加C品和D品;C品滴加时间2h,D品滴加时间2.5h,滴加完毕后,向反应釜中加入氢氧化钠,调节PH值为5.5-6;加入完毕后,保温2-3h后,将温度降至40-45℃,即得减水剂。
实施例3.
配方:甲基烯丙基聚氧乙烯醚30g,丙烯酸3g,巯基乙酸10g,抗坏血酸2g,双氧水12g,氢氧化钠13g,顺丁烯二酸酐3g,亚磷酸钠3g及纯化水制备而成。
工艺:
1、将甲基烯丙基聚氧乙烯醚用纯化水配制成浓度为20%的溶液,得A品;
2、将A品加入反应釜中,加热,直至反应釜内的温度升至60℃,得B品;
3、取滴加罐Ⅰ,依次向滴加罐Ⅰ加入丙烯酸、巯基乙酸、抗坏血酸、顺丁烯二酸酐和亚磷酸钠再向滴加罐Ⅰ加纯化水,使溶液浓度为25%,得C品;
4、取滴加罐Ⅱ,向滴加罐Ⅱ中加入双氧水,再向滴加罐Ⅱ中加纯化水,使溶液浓度为25%,得D品;
5、控制装B品的反应釜内的温度为58-62℃,依次向B品中滴加C品和D品;C品滴加时间2h,D品滴加时间2.5h,滴加完毕后,向反应釜中加入氢氧化钠,调节PH值为5.5-6;加入完毕后,保温2-3h后,将温度降至40-45℃,即得减水剂。
对实施例1所制备的减水剂委托河南省建筑工程质量检验测试中心站有限公司进行检测,检验依据为:GB8076-2008《混泥土外加剂》,检测结果如下:
检验结果,依据GB8076-2008《混泥土外加剂》标准,所检项目符合指标要求。
Claims (1)
1.一种聚羧酸高性能减水剂,其特征在于:按重量份计算,主要由甲基烯丙基聚氧乙烯醚35份,丙烯酸6份,巯基乙酸12份,抗坏血酸2.5份,双氧水2.5份,氢氧化钠15份,顺丁烯二酸酐5份,亚磷酸钠5份及纯化水制备而成;所述的聚羧酸高性能减水剂的制备方法,按下述步骤制备:
(1)将甲基烯丙基聚氧乙烯醚用纯化水配制成浓度为20-25%的溶液,得A品;
(2)将A品加入反应釜中,加热,直至反应釜内的温度升至60℃,得B品;
(3)取滴加罐Ⅰ,依次向滴加罐Ⅰ加入丙烯酸、巯基乙酸、抗坏血酸、顺丁烯二酸酐和亚磷酸钠再向滴加罐Ⅰ加纯化水,使溶液浓度为25-30%,得C品;
(4)取滴加罐Ⅱ,向滴加罐Ⅱ中加入双氧水,再向滴加罐Ⅱ中加纯化水,使溶液浓度为25-30%,得D品;
(5)控制装B品的反应釜内的温度为58-62℃,依次向B品中滴加C品和D品;C品滴加时间为2h,D品滴加时间为2.5h,滴加完毕后,向反应釜中加入氢氧化钠,调节PH值为5-7;加入完毕后,保温2-3h后,将温度降至40-45℃,即得。
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