CN105854818A - 一种气凝胶基消油剂及其制备方法 - Google Patents
一种气凝胶基消油剂及其制备方法 Download PDFInfo
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- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 3
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Abstract
本发明涉及海水治理领域,公开了一种气凝胶基消油剂及其制备方法。制备方法为:a、将正硅酸乙酯、埃洛石粉末、疏水多孔羧甲基纤维素、无水乙醇、甲苯制得溶液A;将无水乙醇、冰醋酸与水制得溶液B;将溶液B滴加到溶液A中;同时向溶液A中添加碳酸氢钠制得溶胶液;b、对溶胶液进行载银操作,制得载银溶胶液;c、将载银溶胶液老化,对载银溶胶液进行溶剂置换后,得到载银凝胶,对载银凝胶进行疏水改性,最后真空干燥后制得气凝胶。本发明制备的气凝胶,在光催化下能够对石油烃进行吸附并降解,且该气凝胶质轻,强度好,孔隙率高,吸油容量大,吸油速率快。
Description
技术领域
本发明涉及海水治理领域,尤其涉及一种气凝胶基消油剂及其制备方法。
背景技术
过去几十年来,我国的工业的快速发展,国民生活水平也不断提高,但是,随着工业的发展,工业对环境的污染也越来越严重。近年来,人们的环保意识逐渐加强,政府对于环境治理也越来越重视。
在众多污染源头中,水污染问题尤为突出,其中,工业油的泄露与排放对海洋、河流造成了巨大的污染,对环境构成了严重的威胁。
目前,一般采用吸油材料对水体中的油进行吸附,最多用到的是高吸油树脂。高吸油树脂是亲油性单体交联而成的聚合物,分子间具有三维交联网络状结构,通过分子内亲油基链段和油分子的溶剂化使树脂发生溶胀作用。由于高吸油树脂只能发生溶胀而不会发生溶解,因此油分子就会负载于三维网状结构中,实现高吸油树脂吸油和保油的功能。
申请号为CN201510692238.X的中国专利公开了一种高吸油树脂及其制备方法,该高吸油树脂包括以下按照重量份数计原料:油相为二乙烯基苯4~8份、苯乙烯20~30份、丙烯酸月桂酯20~30份、丙烯酸丁酯20~30份、顺丁橡胶20~30份、偶氮二异丁腈3~9份、甲苯40~50份;水相为聚乙烯醇5~9份、明胶10~20份、NaCl5~8份、CaCO3 5~10份、去离子水500~600份。
但是高吸油树脂也存在一定的不足之处,比如由于高吸油树脂的孔隙率不够足够高,因此单位质量的高吸油树脂的吸油的容量也受到了一定的限制,并且吸油速率也不够快。此外,高吸油树脂的密度较高,单位体积的树脂较重,也不便于运输、收集等等。最为关键的是,高吸油树脂只能通过物理作用将油品吸附,但是其并不能将油品降解,仍需要回收后等油品进行处理,不仅不方便,也增加了成本。
发明内容
为了解决上述技术问题,本发明提供了一种气凝胶基消油剂及其制备方法。本发明制备的气凝胶,在光催化下能够对石油烃进行吸附并降解,且该气凝胶质轻,强度好,孔隙率高,吸油容量大,吸油速率快。
本发明的具体技术方案为:一种气凝胶基消油剂,所述消油剂的基体为二氧化硅-埃洛石-疏水多孔羧甲基纤维素复合材料,且消油剂的基体上负载有纳米银。
上述的气凝胶基消油剂的制备方法,包括以下步骤:
a、将正硅酸乙酯、埃洛石粉末、疏水多孔羧甲基纤维素、无水乙醇、甲苯按质量比1.5:0.1~0.3:0.05~0.15:10~30:0.01~0.03进行混合,制得溶液A;将无水乙醇、0.5~1.5mol/L的冰醋酸与水按质量比10~20:4~6:1进行混合,制得溶液B;对溶液A在50~60℃下进行超声波振荡处理,将溶液B滴加到3倍质量的溶液A中;同时向溶液A中添加质量为溶液A的0.01~0.02倍的碳酸氢钠粉末,继续搅拌1~2h后,制得溶胶液。
b、向溶胶液中添加质量为正硅酸乙酯0.1~0.3倍的硝酸银并搅拌均匀,接着向溶胶液中滴加硝酸溶液直至溶胶液的pH为5,在避光条件下将溶胶液加热至45~55℃并保温1~2h,对溶胶液用水洗去未反应物质后,在搅拌条件下向溶胶液中添加质量为正硅酸乙酯0.005~0.015倍的硼氢化钠,同时滴加氢氧化钠溶液控制溶胶液pH在7~8之间;最后用水洗涤后制得载银溶胶液。
c、将载银溶胶液在室温下老化24~48h,接着向载银溶胶液中添加正己烷进行溶剂置换36~60h,分离除去正己烷,得到载银凝胶,用有机硅化合物与正己烷的混合溶液对载银凝胶进行疏水改性,最后在60~120℃下真空干燥后制得气凝胶。
传统的气凝胶虽然拥有很高的孔隙率,但是正是由于其孔隙率高,导致其强度较低,骨架特别容易坍塌,不容易成形;并且用作吸油材料时,需要长时间在水面上、光照下漂浮,容易老化而导致性能降低,因此实用性较低。本发明技术方案的气凝胶,采用二氧化硅-埃洛石-疏水多孔羧甲基纤维素的复合材料作为基体骨架,埃洛石为纳米/微米尺寸的无机纤维管,疏水多孔羧甲基纤维素可为市售产品或对自行对多孔羧甲基纤维素进行疏水改性。疏水多孔羧甲基纤维素具有优良的粘结性能,将上述两者与二氧化硅进行掺杂一同制备成气凝胶后,能够大幅地提高气凝胶的强度和耐老化度,延长使用寿命。并且难能可贵的是,由于埃洛石自身也具有纳米/微米尺寸的中空管状结构,与疏水多孔羧甲基纤维素、二氧化硅一同复合后,能够形成复杂的网络状交联结构,并不会过多影响气凝胶的孔隙率,且由于埃洛石的孔隙是自身结构所特有的,并不是通过交联所得,因此强度更高。
在步骤a中,甲苯和碳酸氢钠作为致孔剂,能够在溶胶液的制备过程中致孔,两者的致孔原理不同,相互配合能够制成的较多的孔,因此本气凝胶中含有三种不同成因的孔隙:气凝胶交联形成的孔隙、埃洛石自身的管状孔、致孔剂制成的孔,这三种孔隙尺寸不一,因此能够形成尺寸差异化,对于不同的石油烃,各自的吸附效率也不同,因此能够提高气凝胶的整体吸油效果。
在步骤b中,本发明方法对气凝胶进行了载银,该方法能够提高气凝胶对银的负载牢度,且负载量高。在进行载银后,纳米银在光催化下具有强氧化性,能够使催化石油烃降解。
由于本发明的气凝胶是作为水体的消油剂的,因此需要有较好的亲油性,如此才能实现对石油烃的充分吸收,并且需要避免因吸水而导致容量体积被占据。因此步骤c中,本发明方法对气凝胶进行了疏水改性。
作为优选,所述埃洛石粉末经过改性处理,改性方法为:将埃洛石粉末浸渍于100~200倍质量的10wt%盐酸溶液中,并在50~60℃温度下进行水浴振荡1~2h;将埃洛石粉末取出并洗净后,在400~500℃的马弗炉中煅烧2~5h,最后制得改性埃洛石粉末。经过改性后的埃洛石粉末在改性过程中,去除了内部的结晶水,拓大了其内部容量,具有较高的吸附活性和吸附容量。
作为优选,所述埃洛石粉末的粒径为800~1000nm。该尺寸的埃洛石粉末的中空管与气凝胶中其他两种类型的孔隙进行配合后,能够提高气凝胶的整体吸油性。
作为优选,步骤a中所述正硅酸乙酯、埃洛石粉末、疏水多孔羧甲基纤维素、无水乙醇、甲苯的质量比为1:0.2:0.1:20:0.02;所述无水乙醇、冰醋酸与水的质量比为15:5:1。
作为优选,步骤a中溶液B向溶液A的滴加速度0.5~1.5mL/s。需要严格控制溶液B的滴加速度,该速度下形成溶胶能够形成高交联度的网络状结构,在保证孔隙率的前提下提高强度。
作为优选,步骤c中所述有机硅化合物与正己烷的混合溶液中,有机硅化合物与正己烷的体积比为1~2:5,且有机硅化合物与正己烷的混合溶液与载银凝胶的质量比为100:10~20。
作为优选,步骤c中所述有机硅化合物选自六甲基二硅氧烷、六甲基二硅氮烷、六甲基二硅胺烷、甲基三甲氧基硅烷、三甲基氯硅烷。
作为优选,步骤c中的疏水改性,温度为40~60℃,改性时间为24~48h。
与现有技术对比,本发明的有益效果是:本发明制备的气凝胶,在光催化下能够对石油烃进行吸附并降解,且该气凝胶质轻,强度好,孔隙率高,吸油容量大,吸油速率快。
具体实施方式
下面结合实施例对本发明作进一步的描述。
实施例1
一种气凝胶基消油剂,其制备方法如下:
a、选用粒径为800~1000nm,纯度在98%以上的埃洛石粉末,将埃洛石粉末浸渍于150倍质量的10wt%盐酸溶液中,并在55℃温度下进行水浴振荡1.5h;将埃洛石粉末取出并洗净后,在450℃的马弗炉中煅烧3.5h,最后制得改性埃洛石粉末。
将正硅酸乙酯、改性埃洛石粉末、疏水多孔羧甲基纤维素、无水乙醇、甲苯按质量比1.5:0.2:0.1:20:0.02进行混合,制得溶液A;将无水乙醇、1mol/L的冰醋酸与水按质量比15:5:1进行混合,制得溶液B;对溶液A在55℃下进行超声波振荡处理,将溶液B滴加到3倍质量的溶液A中,控制溶液B的滴加速度1mL/s。同时向溶液A中添加质量为溶液A的0.015倍的碳酸氢钠粉末,继续搅拌1.5h后,制得溶胶液。
b、向溶胶液中添加质量为正硅酸乙酯0.2倍的硝酸银并搅拌均匀,接着向溶胶液中滴加硝酸溶液直至溶胶液的pH为5,在避光条件下将溶胶液加热至50℃并保温1.5h,对溶胶液用水洗去未反应物质后,在搅拌条件下向溶胶液中添加质量为正硅酸乙酯0.01倍的硼氢化钠,同时滴加氢氧化钠溶液控制溶胶液pH在7~8之间;最后用水洗涤后制得载银溶胶液。
c、将载银溶胶液在室温下老化36h,接着向载银溶胶液中添加正己烷进行溶剂置换48h,分离除去正己烷,得到载银凝胶,用有机硅化合物与正己烷的混合溶液对载银凝胶在50℃下进行疏水改性36h,所述有机硅化合物与正己烷的混合溶液中,有机硅化合物与正己烷的体积比为1.5:5,有机硅化合物与正己烷的混合溶液与载银凝胶的质量比为100:15。所述有机硅化合物为六甲基二硅氧烷。最后在90℃下真空干燥后制得气凝胶。
实施例2
一种气凝胶基消油剂,其制备方法如下:
a、选用粒径为800~1000nm,纯度在98%以上的埃洛石粉末,将埃洛石粉末浸渍于100倍质量的10wt%盐酸溶液中,并在50℃温度下进行水浴振荡2h;将埃洛石粉末取出并洗净后,在400℃的马弗炉中煅烧5h,最后制得改性埃洛石粉末。
将正硅酸乙酯、改性埃洛石粉末、疏水多孔羧甲基纤维素、无水乙醇、甲苯按质量比1.5:0.1:0.05:10:0.01进行混合,制得溶液A;将无水乙醇、0.5mol/L的冰醋酸与水按质量比10:4:1进行混合,制得溶液B;对溶液A在50℃下进行超声波振荡处理,将溶液B滴加到3倍质量的溶液A中,控制溶液B的滴加速度0.5mL/s。同时向溶液A中添加质量为溶液A的0.01倍的碳酸氢钠粉末,继续搅拌1h后,制得溶胶液。
b、向溶胶液中添加质量为正硅酸乙酯0.1倍的硝酸银并搅拌均匀,接着向溶胶液中滴加硝酸溶液直至溶胶液的pH为5,在避光条件下将溶胶液加热至45℃并保温2h,对溶胶液用水洗去未反应物质后,在搅拌条件下向溶胶液中添加质量为正硅酸乙酯0.005倍的硼氢化钠,同时滴加氢氧化钠溶液控制溶胶液pH在7~8之间;最后用水洗涤后制得载银溶胶液。
c、将载银溶胶液在室温下老化24h,接着向载银溶胶液中添加正己烷进行溶剂置换36h,分离除去正己烷,得到载银凝胶,用有机硅化合物与正己烷的混合溶液对载银凝胶在40℃下进行疏水改性48h,所述有机硅化合物与正己烷的混合溶液中,有机硅化合物与正己烷的体积比为1:5,有机硅化合物与正己烷的混合溶液与载银凝胶的质量比为100:10。所述有机硅化合物为六甲基二硅氮烷。最后在60℃下真空干燥后制得气凝胶。
实施例3
一种气凝胶基消油剂,其制备方法如下:
a、选用粒径为800~1000nm,纯度在98%以上的埃洛石粉末,将埃洛石粉末浸渍于200倍质量的10wt%盐酸溶液中,并在60℃温度下进行水浴振荡1h;将埃洛石粉末取出并洗净后,在500℃的马弗炉中煅烧2h,最后制得改性埃洛石粉末。
将正硅酸乙酯、改性埃洛石粉末、疏水多孔羧甲基纤维素、无水乙醇、甲苯按质量比1.5:0.3:0.15:30:0.03进行混合,制得溶液A;将无水乙醇、1.5mol/L的冰醋酸与水按质量比20:6:1进行混合,制得溶液B;对溶液A在60℃下进行超声波振荡处理,将溶液B滴加到3倍质量的溶液A中,控制溶液B的滴加速度1.5mL/s。同时向溶液A中添加质量为溶液A的0.02倍的碳酸氢钠粉末,继续搅拌2h后,制得溶胶液。
b、向溶胶液中添加质量为正硅酸乙酯0.3倍的硝酸银并搅拌均匀,接着向溶胶液中滴加硝酸溶液直至溶胶液的pH为5,在避光条件下将溶胶液加热至55℃并保温1h,对溶胶液用水洗去未反应物质后,在搅拌条件下向溶胶液中添加质量为正硅酸乙酯0.015倍的硼氢化钠,同时滴加氢氧化钠溶液控制溶胶液pH在7~8之间;最后用水洗涤后制得载银溶胶液。
c、将载银溶胶液在室温下老化48h,接着向载银溶胶液中添加正己烷进行溶剂置换60h,分离除去正己烷,得到载银凝胶,用有机硅化合物与正己烷的混合溶液对载银凝胶在60℃下进行疏水改性24h,所述有机硅化合物与正己烷的混合溶液中,有机硅化合物与正己烷的体积比为2:5,有机硅化合物与正己烷的混合溶液与载银凝胶的质量比为100:20。所述有机硅化合物为甲基三甲氧基硅烷。最后在120℃下真空干燥后制得气凝胶。
实施例4
一种气凝胶基消油剂,其制备方法如下:
a、选用粒径为800~1000nm,纯度在98%以上的埃洛石粉末,将正硅酸乙酯、埃洛石粉末、疏水多孔羧甲基纤维素、无水乙醇、甲苯按质量比1.5:0.2:0.1:20:0.02进行混合,制得溶液A;将无水乙醇、1mol/L的冰醋酸与水按质量比15:5:1进行混合,制得溶液B;对溶液A在55℃下进行超声波振荡处理,将溶液B滴加到3倍质量的溶液A中,控制溶液B的滴加速度1mL/s。同时向溶液A中添加质量为溶液A的0.015倍的碳酸氢钠粉末,继续搅拌1.5h后,制得溶胶液。
b、向溶胶液中添加质量为正硅酸乙酯0.2倍的硝酸银并搅拌均匀,接着向溶胶液中滴加硝酸溶液直至溶胶液的pH为5,在避光条件下将溶胶液加热至50℃并保温1.5h,对溶胶液用水洗去未反应物质后,在搅拌条件下向溶胶液中添加质量为正硅酸乙酯0.01倍的硼氢化钠,同时滴加氢氧化钠溶液控制溶胶液pH在7~8之间;最后用水洗涤后制得载银溶胶液。
c、将载银溶胶液在室温下老化36h,接着向载银溶胶液中添加正己烷进行溶剂置换48h,分离除去正己烷,得到载银凝胶,用有机硅化合物与正己烷的混合溶液对载银凝胶在50℃下进行疏水改性36h,所述有机硅化合物与正己烷的混合溶液中,有机硅化合物与正己烷的体积比为1.5:5,有机硅化合物与正己烷的混合溶液与载银凝胶的质量比为100:15。所述有机硅化合物为等体积的六甲基二硅胺烷和三甲基氯硅烷。最后在100℃下真空干燥后制得气凝胶。
实施例1~4制得的气凝胶的性能如下表所示:
孔隙率 | 比表面积 | 密度 | 吸油倍率 | 抗拉强度 | |
实施例1 | 94% | 561m2/g | 3.65kg/m3 | 14 | 23.2Gpa |
实施例2 | 92% | 525m2/g | 3.82kg/m3 | 12 | 19.8GPa |
实施例3 | 91% | 502m2/g | 4.12kg/m3 | 12 | 19.4GPa |
实施例4 | 90% | 451m2/g | 4.44kg/m3 | 11 | 20.1GPa |
本发明中所用原料、设备,若无特别说明,均为本领域的常用原料、设备;本发明中所用方法,若无特别说明,均为本领域的常规方法。
以上所述,仅是本发明的较佳实施例,并非对本发明作任何限制,凡是根据本发明技术实质对以上实施例所作的任何简单修改、变更以及等效变换,均仍属于本发明技术方案的保护范围。
Claims (9)
1.一种气凝胶基消油剂,其特征在于:所述消油剂的基体为二氧化硅-埃洛石-疏水多孔羧甲基纤维素复合材料,且消油剂的基体上负载有纳米银。
2.如权利要求1所述的一种气凝胶基消油剂的制备方法,其特征在于包括以下步骤:
a、将正硅酸乙酯、埃洛石粉末、疏水多孔羧甲基纤维素、无水乙醇、甲苯按质量比1.5:0.1~0.3:0.05~0.15:10~30:0.01~0.03进行混合,制得溶液A;将无水乙醇、0.5~1.5mol/L的冰醋酸与水按质量比10~20:4~6:1进行混合,制得溶液B;对溶液A在50~60℃下进行超声波振荡处理,将溶液B滴加到3倍质量的溶液A中;同时向溶液A中添加质量为溶液A的0.01~0.02倍的碳酸氢钠粉末,继续搅拌1~2h后,制得溶胶液;
b、向溶胶液中添加质量为正硅酸乙酯0.1~0.3倍的硝酸银并搅拌均匀,接着向溶胶液中滴加硝酸溶液直至溶胶液的pH为5,在避光条件下将溶胶液加热至45~55℃并保温1~2h,对溶胶液用水洗去未反应物质后,在搅拌条件下向溶胶液中添加质量为正硅酸乙酯0.005~0.015倍的硼氢化钠,同时滴加氢氧化钠溶液控制溶胶液pH在7~8之间;最后用水洗涤后制得载银溶胶液;
c、将载银溶胶液在室温下老化24~48h,接着向载银溶胶液中添加正己烷进行溶剂置换36~60h,分离除去正己烷,得到载银凝胶,用有机硅化合物与正己烷的混合溶液对载银凝胶进行疏水改性,最后在60~120℃下真空干燥后制得气凝胶。
3.如权利要求2所述的一种气凝胶基消油剂的制备方法,其特征在于,所述埃洛石粉末经过改性处理,改性方法为:将埃洛石粉末浸渍于100~200倍质量的10wt%盐酸溶液中,并在50~60℃温度下进行水浴振荡1~2h;将埃洛石粉末取出并洗净后,在400~500℃的马弗炉中煅烧2~5h,最后制得改性埃洛石粉末。
4.如权利要求3所述的一种气凝胶基消油剂的制备方法,其特征在于,所述埃洛石粉末的粒径为800~1000nm。
5.如权利要求2所述的一种气凝胶基消油剂的制备方法,其特征在于,步骤a中所述正硅酸乙酯、埃洛石粉末、疏水多孔羧甲基纤维素、无水乙醇、甲苯的质量比为1.5:0.2:0.1:20:0.02;所述无水乙醇、冰醋酸与水的质量比为15:5:1。
6.如权利要求2所述的一种气凝胶基消油剂的制备方法,其特征在于,步骤a中溶液B向溶液A的滴加速度0.5~1.5mL/s。
7.如权利要求2所述的一种气凝胶基消油剂的制备方法,其特征在于,步骤c中所述有机硅化合物与正己烷的混合溶液中,有机硅化合物与正己烷的体积比为1~2:5,且有机硅化合物与正己烷的混合溶液与载银凝胶的质量比为100:10~20。
8.如权利要求7所述的一种气凝胶基消油剂的制备方法,其特征在于,步骤c中所述有机硅化合物选自六甲基二硅氧烷、六甲基二硅氮烷、六甲基二硅胺烷、甲基三甲氧基硅烷、三甲基氯硅烷。
9.如权利要求8所述的一种气凝胶基消油剂的制备方法,其特征在于,步骤c中的疏水改性,温度为40~60℃,改性时间为24~48h。
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