CN104649364A - 钒硼酸钠在光催化氧化降解氯酚类污染物的方法 - Google Patents
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Abstract
本发明涉及一种钒硼酸钠在光催化氧化降解氯酚类污染物的方法,该方法以氯代苯酚为污染物,在钒硼酸钠的存在下,污染物浓度在10-2000mg/L水溶液,在自然光照射下对其进行降解,20-30分钟内可将其降解50%,在紫外-可见(波长范围320-780nm)及紫外光(254nm)照射下对其进行降解,在5分钟内,脱氯的效率可达97-99%,通过紫外可见光谱仪及高效液相色谱仪分析发现该类氯酚最终降解为小分子羧酸及含氯的溶液。本发明操作工艺简单,成本低,能高效、快速的用于氯代芳烃中的脱氯,对环境保护方面具有良好的前途。
Description
技术领域
本发明涉及一种钒硼酸钠在氯氛类污染中高效快速降解的方法。
背景技术
氯酚类化合物被广泛用作木材的防腐剂、防锈剂、除草剂、杀菌剂和造纸等工业中,具有恶臭、异味和高度毒性,在亚洲、非洲和南美洲还用于血吸虫病的防治,因此在许多工业化国家氯酚的生产规模非常庞大。氯酚类芳香化合物毒性大、难生物降解,具有“三致”效应和遗传毒性,在环境中长期残留、降解周期长,被美国环境保护局列为优先控制污染物。氯酚化合物的大量使用、早期对氯酚危害和毒性的认识不足以及伴随而来的长期忽略,导致氯酚污染非常严重,对人类和环境造成了极大的危害氯酚污染的控制己成为全世界环境学科的研究热点,是环境治理领域的重大课题之一。
氯酚的主要处理方法有生化法、物化法和氧化法等、生化法具有成本低的优点。但由于氯酚毒性大,对微生物有很大影响,处理周期很长,该法对较低浓度的含酚废水处理效果好,对含酚浓度较高、毒性较强的废水的处理效率低。物化法主要包括吸附法、混凝法、萃取法、膜处理技术等,采用物化方法处理氯酚的研究很少,由于物化处理多数伴随着污染物的转移过程,常造成新的污染,需要后续处理过程以达到彻底降解。氧化法可以使化合物的结构发生转变,提高可生化性或直接氧化降解废水中有机物。但装置造价昂贵,催化剂损耗很大。因此,针对氯酚污染物的特点,开发高效、低成本的处理新方法和新技术迫在眉睫。
关于无机钒硼酸钠Na3B6O10VO4的使用在专利号为200810072922.8中已有报道。但其主要是作为钒硼酸钠在非线性光学晶体中的应用,如作为制备非线性光学器件,包括制作倍频发生器、上或下频率转换器和光参量振荡器。本发明提供钒硼酸钠Na3B6O10VO4材料在光催化氧化降解氯酚类污染物方面的方法。同时,在申请号为:201310199066.3的发明中,采用溴硼酸钾在光催化下对氯酚类污染物脱氯的方法,此类虽同属于一类硼酸盐系列,但目标产物及起始原料都不同,此外,本发明中的材料相对溴硼酸钾具有更为优异的光催化性能,其在自然光下对氯酚具有显著的脱氯效果。
发明内容
本发明的目的是提供一种钒硼酸钠材料在光催化氧化降解氯酚类污染物的方法,该方法以氯代苯酚为污染物,在钒硼酸钠的存在下,污染物浓度在10-2000 mg/L水溶液,在自然光照射下对其进行降解,20-30分钟内可将其降解50%,也可在紫外可见(波长范围320-780 nm)及紫外光(254 nm)照射下对其进行降解,在5分钟内,脱氯的效率可达100%,通过紫外可见光谱仪及高效液相色谱仪分析发现该类氯酚最终降解为小分子羧酸及含氯的溶液。本发明操作工艺简单,成本低,能高效、快速的用于氯代芳烃中的脱氯,对环境保护方面具有良好的前途。
本发明所述的一种钒硼酸钠在光催化氧化降解氯酚类污染物的方法,按下列步骤进行:
a、将氯酚溶解在甲醇中,配制成浓度为10g/L的溶液,在溶液中加水稀释至浓度为10-2000mg/L,然后置于超声波中处理60min,使其为均一稳定的溶液;
b、在避光条件下,将钒硼酸钠粉末20-1000 mg加入步骤a溶液中,搅拌30-60分钟,移取4 mL置于离心管内,避光保存;
c、将步骤b中的剩余溶液体系在通风良好的自然光或已经稳定发光的氙灯下辐照,体系温度保持温度25℃,体系距氙灯出口10cm,氙灯光斑直径为50 mm,每间隔时间为0.5-1 min取样4 mL;
d、将所有已经取出的样品离心后取上清液,测试材料的紫外可见吸收光谱、高效液相色谱,分析污染物的降解效率及降解中间产物。
步骤a中所述的氯酚为4-氯酚,2-氯酚,2,4-二氯酚,2,4,6-三氯酚。
步骤c中室温25℃下,自然光能量密度为0.5-2 mw/cm2,氙灯在发射波长420-780 nm,能量密度为1658 mw/cm2。
本发明中含氯酚类可采用市售的原料。
本发明所用的方法为氧化方法,即将一定浓度的代表性氯酚污染物在自然光或不同波长及能量的氙灯照射下,随着时间的变化产生不同浓度自由基,使氯酚类污染物脱氯断链形成小分子羧酸及含氯的溶液。
附图说明
图1是钒硼酸钠粉末衍射XRD图谱;
图2是在钒硼酸钠粉末用量为50mg,2,4-二氯酚浓度50mg/L,分别在自然光、紫外可见光及紫外光照射下的降解效率图,其中-▲-为自然光照射下降解曲线,-●-为波长
320-780 nm照射下降解曲线,-■-为254 nm照射下降解曲线。
具体实施方式
以下结合附图和实施例对本发明进行详细说明:
实施例1:
将2-氯酚溶解在甲醇中使其浓度为10 g/L,取溶解后溶液2 mL,置于容积为250 mL的烧杯中,加水使其稀释至20 mg/L,然后置于超声波中处理60 min,使其为均一稳定的溶液;
在避光条件下,将10mg的钒硼酸钠粉末加入超声波处理后的溶液中,搅拌30分钟,移取4 mL置于离心管内,避光保存;
体系温度保持温度25℃,然后将剩余溶液体系在已经稳定发光的氙灯下辐照,波长为420 nm下辐照,体系距氙灯出口10 cm,氙灯光斑直径为50 mm, 能量密度为1658 mw/cm2,每隔1min时间取样4 mL;
将所有已经取出的样品离心后取上清液,测试材料的紫外可见吸收光谱、高效液相色谱,分析污染物的降解效率及降解中间产物,5分钟后测试2-氯酚脱氯效率为97%,最终产物为小分子羧酸及含氯的溶液。
实施例2:
将2,4-二氯酚溶解在甲醇中使其浓度为10 g/L,取溶解后的溶液0.5 mL,置于容积为250 mL的烧杯中,加水使其稀释至50 mg/L,然后置于超声波中处理60 min,使其为均一稳定的溶液;
在避光条件下,将50 mg的钒硼酸钠粉末加入超声波处理后的溶液中,搅拌30分钟,移取4mL置于离心管内,避光保存;
体系温度保持温度25℃,然后将剩余溶液体系在室温,自然光下辐照,能量密度为0.5-2 mw/cm2,每间隔5 min时间取样4 mL;
将所有已经取出的样品离心后取上清液测试材料的紫外可见吸收光谱、高效液相色谱,分析污染物的降解效率及降解中间产物,20分钟后测试2,4-二氯酚脱氯效率为50%,最终产物为小分子羧酸及含氯的溶液。
实施例3:
将2,4,6-三氯酚溶解在甲醇中使其浓度为10 g/L,取溶解后的溶液5 mL,置于容积为250 mL的烧杯中,加水使其稀释至500 mg/L,然后置于超声波中处理60 min,使其为均一稳定的溶液;
在避光条件下,将50mg的钒硼酸钠粉末加入超声波处理后的溶液中,搅拌40分钟,移取4 mL置于离心管内,避光保存;
体系温度保持室温25 ℃,然后将剩余溶液体系在已经稳定发光的氙灯下辐照,波长为420 nm,体系距氙灯出口10 cm,氙灯光斑直径为50 mm,能量密度为1218 mw/cm2,每间隔0.5 min时间取样4 mL;
将所有已经取出的样品离心后取上清液,测试材料的紫外可见吸收光谱、高效液相色谱,分析污染物的降解效率及降解中间产物,3分钟后测试2,4,6-三氯酚脱氯效率为95%,最终产物为小分子羧酸及含氯的溶液。
实施例4:
将4-氯酚溶解在甲醇中使其浓度为10 g/L,取溶解后的溶液2 mL,置于容积为500 mL的烧杯中,加水使其稀释至200 mg/L,然后置于超声波中处理60 min,使其为均一稳定的溶液;
在避光条件下,将100 mg的钒硼酸钠粉末加入超声波处理后的溶液中,搅拌50分钟,移取4 mL置于离心管内,避光保存;
体系温度保持温度25℃,然后将剩余溶液体系在已经稳定发光的氙灯下辐照,波长为780 nm,体系距氙灯出口10 cm,氙灯光斑直径为50 mm, 能量密度为1658 mw/cm2,每间隔1 min取样4 mL;
将所有已经取出的样品离心后取上清液,测试材料的紫外可见吸收光谱、高效液相色谱,分析污染物的降解效率及降解中间产物,5分钟后测试4-氯酚脱氯效率为98%,最终产物为小分子羧酸及含氯的溶液。
实施例5:
将2,4-二氯酚溶解在甲醇中使其浓度为10 g/L,取溶解后的溶液20 mL,置于容积为1000 mL的烧杯中,加水使其稀释至2000 mg/L,然后置于超声波中处理60 min,使其为均一稳定的溶液;
在避光条件下,将1000mg的钒硼酸钠粉末加入超声波处理后的溶液中,搅拌60分钟,移取4mL置于离心管内,避光保存;
体系温度保持温度25 ℃,然后将剩余溶液体系在已经稳定发光的氙灯下辐照,波长为420 nm,体系距氙灯出口10 cm,氙灯光斑直径为50 mm,能量密度为1218 mw/cm2,每间隔0.5 min取样4 mL;
将所有已经取出的样品离心后取上清液测试材料的紫外可见吸收光谱、高效液相色谱,分析污染物的降解效率及降解中间产物,3分钟后测试2,4-二氯酚脱氯效率为99%,最终产物为小分子羧酸及含氯的溶液。
Claims (3)
1.一种钒硼酸钠在光催化氧化降解氯酚类污染物的方法,其特征在于按下列步骤进行:
a、将氯酚溶解在甲醇中,配制成浓度为10g/L的溶液,在溶液中加水稀释至浓度为10-2000mg/L,然后置于超声波中处理60min,使其为均一稳定的溶液;
b、在避光条件下,将钒硼酸钠粉末20-1000 mg加入步骤a溶液中,搅拌30-60分钟,移取4 mL置于离心管内,避光保存;
c、将步骤b中的剩余溶液体系在通风良好的自然光或已经稳定发光的氙灯下辐照,体系温度保持温度25℃,体系距氙灯出口10 cm,氙灯光斑直径为50 mm,每间隔时间为0.5-1 min取样4 mL;
d、将所有已经取出的样品离心后取上清液,测试材料的紫外可见吸收光谱、高效液相色谱,分析污染物的降解效率及降解中间产物。
2.根据权利要求1所述的方法,其特征在于步骤a中所述的氯酚为4-氯酚,2-氯酚,2,4-二氯酚,2,4,6-三氯酚。
3.根据权利要求1所述的方法,其特征在于步骤c中温度25℃下,自然光能量密度为0.5-2 mw/cm2,氙灯在发射波长420-780 nm,能量密度为1658 mw/cm2。
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