CN107739030A - 一种制备酚醛树脂基泡沫活性炭的方法 - Google Patents
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Abstract
一种制备酚醛树脂基泡沫活性炭的方法,目的是;本发明先将苯酚与37‑40%的甲醛按质量比1:1.1‑3.0混合,在碱性条件中于60‑135℃常压下反应1‑4小时,加入40%‑50%的醋酸调制成中性,并减压脱水得到酚醛树脂;再与发泡剂、表面活性剂、固化剂按照100:10‑20:2‑10:10‑20的比例混合均匀,在40‑100℃下发泡20min‑30min,至体积密度0.04 g/cm3‑0.125g/cm3,形成酚醛泡沫塑料;放入化学活化剂10‑75%的水溶液中浸泡30‑150分钟,然后烘干,使泡沫塑料与活化剂的质量比达到1:4‑5;置于炭化炉中,在氮气体保护下,缓慢升温至300‑400℃,保持1‑4小时;再继续升温到500‑1000℃,进行活化,冷却并除去残留活化剂,得到泡沫活性炭。
Description
技术领域
本发明涉及一种泡沫状活性炭的制备方法。
背景技术
活性炭是黑色的多孔性固体,由于其特殊的结构和优异的吸附性能使得在其很多领域得到了广泛应用。近年来,由于环境问题日益成为世人关注的焦点,活性炭在空气净化、污水处理等方面的独特优势是其它吸附剂所无法替代的,然而以低品位煤炭、纸浆废液、废塑料以及各种废弃的农副产品等为原料制备的性能一般、价格低廉的活性炭已不能满足人们的需要,而以合成树脂、合成纤维为原料,制造具有特殊孔径分布、特殊性能的活性炭日益成为活性炭材料研究的热点。在中国专利CN1303963A所公开了一种制备泡沫块状活性炭纤维的方法,但该方法操作较为复杂,生产成本也比较高。
发明内容
本发明的目的是克服上述已有技术的不足,提供一种收率高、操作方便、环境污染小、孔隙分布均匀且传质阻力小的制备酚醛树脂基泡沫活性炭的方法。
本发明的目的是这样实现的:将液态的酚醛树脂与发泡剂、表面活性剂以及固化剂混合均匀并在一定温度下发泡形成泡沫塑料,然后将其浸渍活化剂,烘干之后在惰性气氛中进行炭化和活化处理,制得泡沫状活性炭。
本发明的具体制备方法如下:
(1)将工业级苯酚与质量百分比浓度37-40%的甲醛按质量比1:1.1-3.0混合,在碱性条件中于60-135℃常压下反应1-4小时,加入质量百分比浓度40%-50%的醋酸调制成中性,并减压至真空度为 0.03 MPa -0.05MPa、温度40℃-90℃;脱水至含水量为10%-15%得到酚醛树脂;所述碱性条件是氢氧化钠与苯酚的质量比为0.01-0.09;
(2)将上述酚醛树脂与发泡剂(液体)、表面活性剂(液体)、固化剂(液体酸)按照质量百分比以100:10-20:2-10:10-20的比例混合均匀,在40-100℃下发泡20min-30min,至体积密度0.04 g/cm3-0.125g/cm3,形成酚醛泡沫塑料;
所述的发泡剂是二氯甲烷、正戊烷、氯仿、四氯化碳、环己烷中的任意一种;
所述的表面活性剂是硅烷和吐温系列表面活性剂中的任意一种;
所述的固化剂是盐酸、硫酸、磷酸、酚磺酸、甲基苯磺酸中的任意一种;所述的固化剂的质量百分比浓度为35-40%;
(3)将化学活化剂配成质量百分比浓度10-75%的水溶液,将上述酚醛泡沫塑料在活化剂溶液中浸泡30-150分钟,然后将其烘干,使泡沫塑料与活化剂(干粉)的质量比达到泡沫塑料:活化剂=1:4-5;
所述化学活化剂是氢氧化钾、碳酸钾、氯化锌、氯化铜、硝酸、硝酸盐、磷酸、偏磷酸中的任意一种;
(4)将含有活化剂的泡沫塑料置于炭化炉中,在氮气体保护下,缓慢升温至300-400℃,保持1-4小时;再继续升温到500-1000℃,进行活化时间为0.5-4小时,然后在氮气气氛中冷却至室温,水洗除去残留活化剂,得到泡沫活性炭。
炭化炉为Ф80的电热管式炭化炉。所述的炭化炉中的氮气体保护条件是流量1 l/min -3l/min、按气体体积计的99.5%为氮气,压力为500Pa。所述的炭化炉中的氮气气氛条件为流量1l/min-3l/min,按气体体积计的99.5%为氮气,压力为500Pa。
本发明与已有的技术相比具有如下优点:
1.以酚醛泡沫塑料做为活性炭前驱体,与其它原料相比,由于酚醛树脂具有确定的大分子结构,杂质含量少或几乎不含杂质,所以其衍生的活性炭具有孔径分布的可控性和性能的可重复性,同时,以酚醛树脂为原料制备活性炭时其炭化收率高;
2.以多聚甲醛为原料合成酚醛树脂时,无须脱水,既操作方便又减少了废水对环境的污染。采用不含氯氟烃的发泡剂减少了对大气的污染;
3.通过调节酚醛泡沫塑料的孔结构可以达到控制活性炭空隙率的目的,所得到的活性炭具有固定的形状和很好的吸附性能,比表面积大、孔隙分布均匀且传质阻力小,易于工程化应用;
4.与CN1303963A所公开的方法相比,本发明制备工艺简单,易操作,成本低廉。
具体实施方式
实施例1:
本发明方法是:
(1)在带有搅拌器和回流冷凝管的100ml三口烧瓶中加入25g苯酚和40ml37%甲醛水溶液以及0.55g氢氧化钠,缓慢升温,待苯酚溶解之后开动搅拌器,使其在80℃下反应3小时,反应液达到终点后,用50%的醋酸溶液中和,然后在50℃左右进行减压脱水,使其含水量为15%左右,得到红棕色液态可发性酚醛树脂。
(2)在20g酚醛树脂中加入3ml二氯甲烷、0.5mlTwwen60,将其搅拌均匀后,加入4ml50%的浓硫酸,快速搅拌10-30秒,然后注入模具,在80℃下发泡、熟化0.5小时,可制得孔径分布均匀且开孔率高的泡沫塑料。
(3)将10g泡沫塑料与氢氧化钾溶液混合浸渍,保持泡沫塑料:活化剂=1:4,120℃烘干。
(4)将含有活化剂的泡沫塑料置于炭化炉中,在惰性气体保护下,缓慢升温至300℃,保持1小时,继续升温到800℃,进行活化2.5小时,然后在惰性气氛中冷却至室温,水洗除去残留活化剂,即得泡沫活性炭。
实施例2:
本发明方法是:
(1)将苯酚与甲醛按1:1.1-3的比例混合,在碱性条件中于60-135℃下反应1-4小时,中和并减压脱水得到酚醛树脂。
(2)将上述酚醛树脂与发泡剂、表面活性剂、固化剂以100:10-20:2-10:10-20(质量份)的比例混合均匀,在40-100℃下发泡形成酚醛泡沫塑料。
(3)将化学活化剂配成10-75%的水溶液,将酚醛泡沫塑料在活化剂溶液中浸泡30-150分钟,然后将其烘干,使泡沫塑料与活化剂的质量比为泡沫塑料:活化剂=1:2-5。
(4)将含有活化剂的泡沫塑料置于炭化炉中,在惰性气体保护下,缓慢升温至300-400℃,保持1-4小时,继续升温到500-1000℃,进行活化0.5-4小时,然后在惰性气氛中冷却至室温,水洗除去残留活化剂,即得泡沫活性炭。
上述的发泡剂是二氯甲烷、正戊烷、氯仿、四氯化碳、环己烷中的任意一种。上所述的表面活性剂是硅烷和吐温系列表面活性剂中的任意一种。上所述的固化剂是盐酸、硫酸、磷酸、酚磺酸、甲基苯磺酸及其混合酸中的任意一种。上所述的化学活化剂是氢氧化钾、碳酸钾、氯化锌、氯化铜、硝酸、硝酸盐、磷酸、偏磷酸及其盐中的任意一种。
Claims (4)
1.一种制备酚醛树脂基泡沫活性炭的方法,其特征在于:
(1)将工业级苯酚与质量百分比浓度37-40%的甲醛按质量比1:1.1-3.0混合,在碱性条件中于60-135℃常压下反应1-4小时,加入质量百分比浓度40%-50%的醋酸调制成中性,并减压至真空度为 0.03 MPa -0.05MPa、温度40℃-90℃;脱水至含水量为10%-15%得到酚醛树脂;所述碱性条件是氢氧化钠与苯酚的质量比为0.01-0.09;
(2)将上述酚醛树脂与发泡剂(纯液体)、表面活性剂(纯液体)、固化剂(37%液体酸)按照质量百分比以100:10-20:2-10:10-20的比例混合均匀,在40-100℃下发泡20min-30min,至体积密度0.04 g/cm3-0.125g/cm3,形成酚醛泡沫塑料;
所述的发泡剂是二氯甲烷、正戊烷、氯仿、四氯化碳、环己烷中的任意一种;
所述的表面活性剂是硅烷和吐温系列表面活性剂中的任意一种;
所述的固化剂是盐酸、硫酸、磷酸、酚磺酸、甲基苯磺酸中的任意一种;质量百分比浓度为35-40%;
(3)将化学活化剂配成质量百分比浓度10-75%的水溶液,将上述酚醛泡沫塑料在活化剂溶液中浸泡30-150分钟,然后将其烘干,使泡沫塑料与活化剂(干粉)的质量比达到泡沫塑料:活化剂=1:4-5;
所述化学活化剂是氢氧化钾、碳酸钾、氯化锌、氯化铜、硝酸、硝酸盐、磷酸、偏磷酸中的任意一种;
(4)将含有活化剂的泡沫塑料置于炭化炉中,在氮气体保护下,缓慢升温至300-400℃,保持1-4小时;再继续升温到500-1000℃,进行活化时间为0.5-4小时,然后在氮气气氛中冷却至室温,水洗除去残留活化剂,得到泡沫活性炭。
2.根据权利要求1所述的制备酚醛树脂基泡沫活性炭的方法,其特征在于炭化炉为Ф80的电热管式炭化炉。
3.根据权利要求1或2或所述的制备酚醛树脂基泡沫活性炭的方法,其特征在于所述的炭化炉中的氮气体保护条件是流量1 l/min -3l/min、按气体体积计的99.5%为氮气,压力为500Pa。
4.根据权利要求1或2或所述的制备酚醛树脂基泡沫活性炭的方法,其特征在于所述的炭化炉中的氮气气氛条件为流量1l/min-3l/min,按气体体积计的99.5%为氮气,压力为500Pa。
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CN115739178B (zh) * | 2022-09-08 | 2024-03-26 | 河北科技大学 | 一种酚醛泡沫负载锰铁氧体催化剂的制备方法及其用途 |
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