CN107129707A - 聚硫密封胶专用纳米碳酸钙的制备方法 - Google Patents
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Abstract
本发明公开了一种聚硫密封胶专用纳米碳酸钙的制备方法,按照以下步骤实施:①制浆;②调浆;③碳化;④表面处理;⑤表面处理后的碳酸钙熟浆经压滤、干燥、粉碎,将BET比表面积控制为15~30m2/g,制得水分≤0.3%的硫密封胶专用纳米碳酸钙。应用本发明制备的纳米碳酸钙用于聚硫密封胶时能使其具有更好的触变特性、补强性能、拉伸性能和加工性能,延长可以操作的工作时间,提高聚硫密封胶对各种材料的附着力,更好地满足使用需求。
Description
技术领域
本发明涉及纳米碳酸钙生产技术领域,具体涉及一种聚硫密封胶专用纳米碳酸钙的制备方法。
背景技术
聚硫密封胶是以液态聚硫橡胶为基体,配合增塑剂、填料、偶联剂、补强剂、硫化剂、促进剂等助剂而制成。液体聚硫胶主链上含有-S-S-链,端基为-SH,如使-SH发生反应可产生固化,从而形成高分子量的聚硫橡胶。由于其分子链是饱和的,且在主链上含有硫原子,因而具有良好的耐老化性能,同时分子链末端含有活泼的硫醇基,常温下与金属过氧化物发生固化反应。聚硫密封胶具有固化均匀、耐药品性强、耐候性好等优点,是一类性能优异的弹性密封材料。与湿固化的硅酮密封胶、聚氨酯胶相比,可控性好,利于施工操作,因此广泛用于土木建筑、汽车制造等行业作为嵌缝、密封材料,还常用于各类油箱、燃料罐、航空机械、复合玻璃的密封。
在各类工业应用中,聚硫密封胶需要有良好的触变性和机械性能,虽然可以通过化学改性和加入触变剂(如白炭黑)的方法来解决此类问题,但是化学改性工艺复杂,使制造成本升高,难以大规模化;而白炭黑虽然可有效提高胶料触变性,但与此同时也会造成加工困难,生产消耗能量巨大。
选用合适的填料是极有效的物理改性手段,可以保证聚硫胶具有必要的强度,又要确保其经济性。纳米碳酸钙作为一种经济型的纳米材料,价格较低,性能优良,广泛用于橡胶、电线、密封胶、油墨、汽车涂料等行业。但是目前国内市售的纳米碳酸钙产品,用于聚硫密封胶时加工性能和触变性都不理想,可操作时间短,力学性能差,拉伸粘结性能低,难以满足高性能的要求。
发明内容
本发明所解决的技术问题是提供一种硫密封胶专用纳米碳酸钙的制备方法,应用本发明制备的纳米碳酸钙用于聚硫密封胶时能使其具有更好的触变特性、补强性能、拉伸性能和加工性能,延长可以操作的工作时间,提高聚硫密封胶对各种材料的附着力,更好地满足使用需求。
本发明所采用的技术方案是:聚硫密封胶专用纳米碳酸钙的制备方法,按照以下步骤实施:
①制浆:将石灰石破碎成直径为4~8cm的颗粒,经煅烧得到氧化钙,然后加水消化生成Ca(OH)2,Ca(OH)2经过精制陈化12~48h,过筛得到Ca(OH)2浆料;
②调浆:调节Ca(OH)2浆料的温度为10~30℃,质量百分浓度为9~12%,加入乳化剂OP-10,OP-10与Ca(OH)2浆料的重量比为(0.1~0.3)︰100,然后泵入带搅拌器的碳化塔中;
③碳化:开启搅拌,同时向碳化塔中通入CO2体积含量为28~35%的窑气与Ca(OH)2浆料进行碳化反应,当碳化到pH=7~8时,停止CO2气体的通入,制得碳酸钙熟浆;
④表面处理:将碳酸钙熟浆输送至表面处理罐,加热到60~75℃,然后加入表面处理剂,表面处理剂与熟浆中碳酸钙固含量的重量比为(3~6)︰100,继续搅拌1~2小时;所述表面处理剂的组成为:按重量百分含量计,棕榈仁油40~70%、Si-69硅烷偶联剂30~60%;所述表面处理剂加入到碳酸钙熟浆前加热到80~95℃;
⑤表面处理后的碳酸钙熟浆经压滤、干燥、粉碎,将BET比表面积控制为15~30m2/g,制得水分≤0.3%的硫密封胶专用纳米碳酸钙。
步骤②中所述OP-10与Ca(OH)2浆料的重量比优选为0.2︰100。
步骤④中所述表面处理剂与熟浆中碳酸钙固含量的重量比优选为4.5︰100,所述表面处理剂的组成优选为:按重量百分含量计,棕榈仁油60%、Si-69硅烷偶联剂40%。
本发明的有益效果是:1、本发明在碳化过程中,加入乳化剂OP-10,该乳化剂是一种烷基酚与环氧乙烷的缩合物,属于非离子型表面活性剂,能增加反应界面的表面积,可以提高碳化反应速度,使CO2和Ca(OH)2之间的反应剧烈,使溶液在极短的时间内形成很高的饱和度,促进了大量的CaCO3粒子均相成核,成核速度快,而且数目多,生成的CaCO3粒子非常细小且均匀,同时有包覆作用提高分散性;2、本发明采用棕榈仁油和Si-69硅烷偶联剂的混合物进行表面处理,棕榈仁油主要从棕榈的内核提取,是一类含12-18C的脂肪酸甘油脂,熔点为24~26℃,熔点合适,其碘值(g碘/100g油)为14~22,较棕榈油低,具有良好的热稳定性,进行湿法表面处理时,有利于在纳米碳酸钙界面包覆,形成定向的排列,提高纳米碳酸钙的分散性,使之不团聚,从而增加纳米碳酸钙的分散稳定性,降低吸油值,可作为粘度控制剂,提高触变性,延长可以操作的工作时间;而Si-69硅烷偶联剂可以提高聚硫胶的强度和拉伸性能,4个S原子还可起硫化促进作用,提高耐老化性能和贮存稳定性;3、本发明制备的纳米碳酸钙具有良好的加工性能,可以提高聚硫密封胶的触变性和抗流挂性,而且具有良好的补强和拉伸性能,对各种铝材、玻璃、水泥等材料具有优异的附着力;4、本发明制备的纳米碳酸钙的BET比表面积控制在15-30m2/g,当BET比表面积超过30m2/g时,比表面积太大,粒子太小,可施工的时间变短,粘度大,难以操作;当BET小于15m2/g时,比表面积太小,粒子太大,力学性能变差,触变性变差。
具体实施方式
下面结合具体实施例对本发明做进一步说明。
实施例1:
聚硫密封胶专用纳米碳酸钙的制备方法,按照以下步骤实施:
①制浆:将石灰石破碎成直径为4~8cm的颗粒,经煅烧得到氧化钙,然后加水消化生成Ca(OH)2,Ca(OH)2经过精制陈化12h,过筛得到Ca(OH)2浆料;
②调浆:调节Ca(OH)2浆料的温度为15℃,质量百分浓度为9%,加入乳化剂OP-10,OP-10与Ca(OH)2浆料的重量比为0.1︰100,然后泵入带搅拌器的碳化塔中;
③碳化:开启搅拌,同时向碳化塔中通入CO2体积含量为28%的窑气与Ca(OH)2浆料进行碳化反应,当碳化到pH=7~8时,停止CO2气体的通入,制得碳酸钙熟浆;
④表面处理:将碳酸钙熟浆输送至表面处理罐,加热到60~75℃,然后加入表面处理剂,表面处理剂与熟浆中碳酸钙固含量的重量比为3︰100,继续搅拌1小时;所述表面处理剂的组成为:按重量百分含量计,棕榈仁油40%、Si-69硅烷偶联剂60%;所述表面处理剂加入到碳酸钙熟浆前加热到80~95℃;
⑤表面处理后的碳酸钙熟浆经压滤、干燥、粉碎,制得BET比表面积为18.58m2/g,水分≤0.3%的硫密封胶专用纳米碳酸钙。
实施例2
聚硫密封胶专用纳米碳酸钙的制备方法,按照以下步骤实施:
①制浆:将石灰石破碎成直径为4~8cm的颗粒,经煅烧得到氧化钙,然后加水消化生成Ca(OH)2,Ca(OH)2经过精制陈化48h,过筛得到Ca(OH)2浆料;
②调浆:调节Ca(OH)2浆料的温度为30℃,质量百分浓度为12%,加入乳化剂OP-10,OP-10与Ca(OH)2浆料的重量比为0.3︰100,然后泵入带搅拌器的碳化塔中;
③碳化:开启搅拌,同时向碳化塔中通入CO2体积含量为35%的窑气与Ca(OH)2浆料进行碳化反应,当碳化到pH=7~8时,停止CO2气体的通入,制得碳酸钙熟浆;
④表面处理:将碳酸钙熟浆输送至表面处理罐,加热到60~75℃,然后加入表面处理剂,表面处理剂与熟浆中碳酸钙固含量的重量比为6︰100,继续搅拌2小时;所述表面处理剂的组成为:按重量百分含量计,棕榈仁油70%、Si-69硅烷偶联剂30%;所述表面处理剂加入到碳酸钙熟浆前加热到80~95℃;
⑤表面处理后的碳酸钙熟浆经压滤、干燥、粉碎,制得BET比表面积为26.62m2/g、水分≤0.3%的硫密封胶专用纳米碳酸钙。
实施例3
聚硫密封胶专用纳米碳酸钙的制备方法,按照以下步骤实施:
①制浆:将石灰石破碎成直径为4~8cm的颗粒,经煅烧得到氧化钙,然后加水消化生成Ca(OH)2,Ca(OH)2经过精制陈化30h,过筛得到Ca(OH)2浆料;
②调浆:调节Ca(OH)2浆料的温度为20℃,质量百分浓度为11%,加入乳化剂OP-10,OP-10与Ca(OH)2浆料的重量比为0.2︰100,然后泵入带搅拌器的碳化塔中;
③碳化:开启搅拌,同时向碳化塔中通入CO2体积含量为31%的窑气与Ca(OH)2浆料进行碳化反应,当碳化到pH=7~8时,停止CO2气体的通入,制得碳酸钙熟浆;
④表面处理:将碳酸钙熟浆输送至表面处理罐,加热到60~75℃,然后加入表面处理剂,表面处理剂与熟浆中碳酸钙固含量的重量比为4.5︰100,继续搅拌1.5小时;所述表面处理剂的组成为:按重量百分含量计,棕榈仁油60、Si-69硅烷偶联剂40%;所述表面处理剂加入到碳酸钙熟浆前加热到80~95℃;
⑤表面处理后的碳酸钙熟浆经压滤、干燥、粉碎,制得BET比表面积为22.4m2/g、水分≤0.3%的硫密封胶专用纳米碳酸钙。
Claims (3)
1.聚硫密封胶专用纳米碳酸钙的制备方法,其特征在于,按照以下步骤实施:
①制浆:将石灰石破碎成直径为4~8cm的颗粒,经煅烧得到氧化钙,然后加水消化生成Ca(OH)2,Ca(OH)2经过精制陈化12~48h,过筛得到Ca(OH)2浆料;
②调浆:调节Ca(OH)2浆料的温度为10~30℃,质量百分浓度为9~12%,加入乳化剂OP-10,OP-10与Ca(OH)2浆料的重量比为(0.1~0.3)︰100,然后泵入带搅拌器的碳化塔中;
③碳化:开启搅拌,同时向碳化塔中通入CO2体积含量为28~35%的窑气与Ca(OH)2浆料进行碳化反应,当碳化到pH=7~8时,停止CO2气体的通入,制得碳酸钙熟浆;
④表面处理:将碳酸钙熟浆输送至表面处理罐,加热到60~75℃,然后加入表面处理剂,表面处理剂与熟浆中碳酸钙固含量的重量比为(3~6)︰100,继续搅拌1~2小时;所述表面处理剂的组成为:按重量百分含量计,棕榈仁油40~70%、Si-69硅烷偶联剂30~60%;所述表面处理剂加入到碳酸钙熟浆前加热到80~95℃;
⑤表面处理后的碳酸钙熟浆经压滤、干燥、粉碎,将BET比表面积控制为15~30m2/g,制得水分≤0.3%的硫密封胶专用纳米碳酸钙。
2.根据权利要求1所述的聚硫密封胶专用纳米碳酸钙的制备方法,其特征在于,步骤②中所述OP-10与Ca(OH)2浆料的重量比为0.2︰100。
3.根据权利要求1所述的聚硫密封胶专用纳米碳酸钙的制备方法,其特征在于,步骤④中所述表面处理剂与熟浆中碳酸钙固含量的重量比为4.5︰100,所述表面处理剂的组成为:按重量百分含量计,棕榈仁油60%、Si-69硅烷偶联剂40%。
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