CN115073678A - 一种高适应性醚类聚羧酸及其制备方法 - Google Patents
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Abstract
一种高适应性醚类聚羧酸及其制备方法,本发明公开了一种高适应性醚类聚羧酸。所述制备方法包括以下步骤:(1)将异戊烯醇聚氧乙烯醚和水加热搅拌后,先加入α‑甲基丙烯酸反应,再滴加硫代乙醇酸反应后,再加入聚乙二醇混合,得A组分;(2)将双氧水、过硫酸铵和维生素C混合溶解后,得B组分;(3)将步骤(2)所得B组分滴入步骤(1)所得A组分中,反应后,调节pH值,得高适应性醚类聚羧酸。本发明高适应性醚类聚羧酸适应性很高,与硅酸盐水泥及各类辅助性胶凝材料的相容性好。本发明制备方法可在常温下进行,工艺简单,成本低,适宜于工业化生产。
Description
技术领域
本发明涉及一种聚羧酸及其制备方法,具体涉及一种高适应性醚类聚羧酸及其制备方法。
背景技术
聚羧酸(PCE)作为新一代混凝土减水剂,具有分子设计自由度大、原料来源范围广、减水率较高等优点,普通聚羧酸的结构如下所示:
分子设计中,侧链大单体结构对聚羧酸的吸附性、减水率、保坍性等性能和作用机理有着至关重要的影响,应重点考虑。
以下是普通聚羧酸的反应式,是由丙烯酸(主链)聚合之后,侧链大单体接枝进入主链的侧链大单体,此类大单体可为氨脂类大单体,没有碳碳双键,因此缩合进入。
还有一种醚类大单体,有双键,可以直接脱去双键,进入主链。
聚羧酸减水剂分子中含有很多官能团,这些基团能吸附于硅酸盐水泥的水化产物和其颗粒的表面,不仅可形成吸附层,而且可破坏硅酸盐颗粒间的絮凝结构。聚羧酸减水剂掺入后,其静电斥力和空间位阻等作用能极大改变硅酸盐水泥颗粒间的作用力及其固-液界面的物化性能,使硅酸盐水泥颗粒分布均匀,进而影响水泥浆体的流动度及其它性能,但现有聚羧酸减水剂用于硅酸盐水泥后其适应性不好。聚羧酸的设计合成中,为增大其相容性,一般都是引入各种基团,如:减缩基团,保塌基团,引气基团等,但是,这样加入之后结构复杂,合成困难,成本高。
另外,目前合成聚羧酸减水剂通常采用的是加热合成,合成温度在60~90℃之间,有的甚至更高,合成的减水剂相对含固量较低,这样一来在合成以及运输的过程中,无意间增加合成聚羧酸减水剂的合成和销售成本,常温合成聚羧酸减水剂已成为减水剂行业的发展一种趋势。
发明内容
本发明所要解决的技术问题是,克服现有技术存在的上述缺陷,提供一种适应性很高,与硅酸盐水泥及各类辅助性胶凝材料的相容性好的高适应性醚类聚羧酸。
本发明进一步要解决的技术问题是,克服现有技术存在的上述缺陷,提供一种可在常温下进行,工艺简单,成本低,适宜于工业化生产的高适应性醚类聚羧酸的制备方法。
本发明解决其技术问题所采用的技术方案如下:一种高适应性醚类聚羧酸,所述高适应性醚类聚羧酸的结构式为:
,a为1~40、b为1~40、d为1~800、e为1~800、f为1~800、g为1~800。本发明高适应性醚类聚羧酸吸附在水泥颗粒上,可阻碍水和离子在水泥矿物与孔隙溶液界面的平滑扩散,由Ca2+和COO-形成的螯合作用抑制了水化物产物的成核和沉淀,增加了分子上的吸附位点的数量,并且水泥颗粒可以更好地包裹并分散在溶液中。
本发明进一步解决其技术问题所采用的技术方案如下:一种高适应性醚类聚羧酸的制备方法,包括以下步骤:
(1)将异戊烯醇聚氧乙烯醚和水加热搅拌后,先加入α-甲基丙烯酸反应,再滴加硫代乙醇酸反应后,再加入聚乙二醇混合,得A组分;
(2)将双氧水、过硫酸铵和维生素C混合溶解后,得B组分;
(3)将步骤(2)所得B组分滴入步骤(1)所得A组分中,反应后,调节pH值,得高适应性醚类聚羧酸。
本发明制备方法中,双氧水和维生素C会发生化学反应产生一定数量的自由基和热量,在所述温度下即可链引发整个高分子反应,因此实现常温聚合。
本发明制备方法的反应方程式如下所示:
优选地,步骤(1)中,异戊烯醇聚氧乙烯醚与α-甲基丙烯酸的摩尔比为1:1~3。更优选地,所述异戊烯醇聚氧乙烯醚的分子量为2160~10000。
优选地,步骤(1)中,所述异戊烯醇聚氧乙烯醚与水的质量比为1:0.5~1.0。
优选地,步骤(1)中,所述加热搅拌的温度为40~60℃,时间为1~3h。
优选地,步骤(1)中,所述加入α-甲基丙烯酸反应的温度为40~60℃,时间为0.5~1.5h。
优选地,步骤(1)中,所述硫代乙醇酸与α-甲基丙烯酸的质量比为0.02~0.20:1。
优选地,步骤(1)中,滴加硫代乙醇酸后反应的温度为40~60℃,时间为0.5~1.5h。
优选地,步骤(1)中,所述聚乙二醇与α-甲基丙烯酸的质量比为0.2~0.8:1。更优选地,所述聚乙二醇的分子量为200~1000。
优选地,步骤(2)中,所述双氧水、过硫酸铵和维生素C的摩尔比为10~20:0.5~1.5:1。所述双氧水的质量分数为20~30%。
优选地,步骤(3)中,所述B组分与A组分的质量比为2~5:100。
优选地,步骤(3)中,所述B组分滴入的时间为1~10min。
优选地,步骤(3)中,所述反应的温度为40~60℃,时间为1~4h。
优选地,步骤(3)中,所述调节pH值至6~7。用NaOH调节pH值。
本发明方法的有益效果如下:
(1)本发明高适应性醚类聚羧酸适应性很高,与硅酸盐水泥及各类辅助性胶凝材料的相容性好;
(2)本发明制备方法可在常温下进行,工艺简单,成本低,适宜于工业化生产。
具体实施方式
下面结合实施例对本发明作进一步说明。
本发明实施例所使用的双氧水的质量分数为30%;本发明实施例所使用的原料或化学试剂,如无特殊说明,均通过常规商业途径获得。
一种高适应性醚类聚羧酸实施例1
所述高适应性醚类聚羧酸的结构式为:
一种高适应性醚类聚羧酸的制备方法实施例1
(1)将0.05mol(120g)异戊烯醇聚氧乙烯醚2400和100g水,在45℃下,加热搅拌1.5h后,先加入0.15mol(12.91g)α-甲基丙烯酸在45℃下,反应1.5h,再滴加1.9365g硫代乙醇酸在45℃下,反应1.5h后,再加入8g聚乙二醇400混合,得230g A组分;
(2)将0.06mol(6.8g)双氧水、0.004mol(0.91g)过硫酸铵和0.003mol(0.53g)维生素C混合溶解后,得8.24g B组分;
(3)将步骤(2)所得8.24g B组分以滴加时间为5min,滴入步骤(1)所得230g A组分中,在45℃下,反应1h后,用NaOH调节pH值至7,得高适应性醚类聚羧酸(记为M-PCE)。
一种高适应性醚类聚羧酸实施例2
所述高适应性醚类聚羧酸的结构式为:
一种高适应性醚类聚羧酸的制备方法实施例2
(1)将0.05mol(120g)异戊烯醇聚氧乙烯醚2400和80g水,在50℃下,加热搅拌1h后,先加入0.1mol(8.61g)α-甲基丙烯酸在50℃下,反应1h,再滴加0.9212g硫代乙醇酸在50℃下,反应1h后,再加入4g聚乙二醇400混合,得200g A组分;
(2)将0.05mol(5.67g)双氧水、0.003mol(0.76g)过硫酸铵和0.003mol(0.59g)维生素C混合溶解后,得7.0g B组分;
(3)将步骤(2)所得7.0g B组分以滴加时间为4min,滴入步骤(1)所得200g A组分中,在50℃下,反应3h后,用NaOH调节pH值至7,得高适应性醚类聚羧酸(记为O-PCE)。
将葡萄糖酸钠、柠檬酸、酒石酸、六偏磷酸钠、白糖按3:1:1:1:4的比例混合,再分别按M-PCE、O-PCE的总掺量为5%进行复配,即得聚羧酸减水剂M-PCE、O-PCE。
分别将15g M-PCE、O-PCE和市售普通聚羧酸盐C-PCE-1、C-PCE-2与100g水泥混合后,对其分散性进行测试,结果如表1所示。
表1 本发明M-PCE、O-PCE和市售普通聚羧酸减水剂C-PCE-1、C-PCE-2的分散性测试结果表
由表1可知,不同TPEG与丙烯酸摩尔比制得的减水剂产品在净浆流动度上存在一定差异,随着时间的延长净浆流动度差值会变得越来越大,M-PCE减水剂在表面张力与净浆流动度两方面的性能最优,由此亦可知,相同条件下,增加TPEG的量可以显著提升减水剂的性能。
Claims (5)
2.一种如权利要求1所述高适应性醚类聚羧酸的制备方法,其特征在于,包括以下步骤:
(1)将异戊烯醇聚氧乙烯醚和水加热搅拌后,先加入α-甲基丙烯酸反应,再滴加硫代乙醇酸反应后,再加入聚乙二醇混合,得A组分;
(2)将双氧水、过硫酸铵和维生素C混合溶解后,得B组分;
(3)将步骤(2)所得B组分滴入步骤(1)所得A组分中,反应后,调节pH值,得高适应性醚类聚羧酸。
3.根据权利要求2所述高适应性醚类聚羧酸的制备方法,其特征在于:步骤(1)中,异戊烯醇聚氧乙烯醚与α-甲基丙烯酸的摩尔比为1:1~3;所述异戊烯醇聚氧乙烯醚与水的质量比为1:0.5~1.0;所述加热搅拌的温度为40~60℃,时间为1~3h;所述加入α-甲基丙烯酸反应的温度为40~60℃,时间为0.5~1.5h;所述硫代乙醇酸与α-甲基丙烯酸的质量比为0.02~0.20:1;滴加硫代乙醇酸后反应的温度为40~60℃,时间为0.5~1.5h;所述聚乙二醇与α-甲基丙烯酸的质量比为0.2~0.8:1。
4.根据权利要求2或3所述高适应性醚类聚羧酸的制备方法,其特征在于:步骤(2)中,所述双氧水、过硫酸铵和维生素C的摩尔比为10~20:0.5~1.5:1。
5.根据权利要求2或3所述高适应性醚类聚羧酸的制备方法,其特征在于:步骤(3)中,所述B组分与A组分的质量比为2~5:100;所述B组分滴入的时间为1~10min;所述反应的温度为40~60℃,时间为1~4h;所述调节pH值至6~7。
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