CN103936136A - Treatment method of trivalent arsenic in oxalic acid oxidized water body by ultraviolet excitation - Google Patents
Treatment method of trivalent arsenic in oxalic acid oxidized water body by ultraviolet excitation Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 24
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
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Abstract
Description
技术领域 technical field
本发明涉及污水处理领域，特别涉及一种利用紫外光激发草酸氧化水体中三价砷的处理方法。 The invention relates to the field of sewage treatment, in particular to a treatment method for using ultraviolet light to excite oxalic acid to oxidize trivalent arsenic in water.
背景技术 Background technique
砷(As)是一种在地壳中广泛分布的元素，并被公认为一种有毒的致癌物质。As的化合物有三价和五价两种形态，As(III)的毒性和流动性更大。研究表明，以AsO3 3-存在的As(III)比以AsO4 3-存在的As(V)的毒性要高出60倍。砷化物在采矿、冶炼、玻璃制造、农药和木材防腐剂等生产领域得到广泛应用的同时，致使相当数量的砷化合物进入环境，并通过化学过程和生物转化效应以不同形态存在于水体、土壤、植物、动物、海洋生物和人体内，并且在各砷化物之间形成循环。 Arsenic (As) is an element widely distributed in the earth's crust and is recognized as a toxic carcinogen. As compounds have trivalent and pentavalent forms, and As(III) is more toxic and mobile. Studies have shown that the toxicity of As(III) in the form of AsO 3 3- is 60 times higher than that of As(V) in the form of AsO 4 3- . While arsenic compounds are widely used in production fields such as mining, smelting, glass manufacturing, pesticides and wood preservatives, a considerable amount of arsenic compounds enters the environment and exists in water, soil, plants, animals, marine organisms and humans, and forms a cycle between the various arsenic compounds.
根据世界卫生组织的研究，只要在饮用水中出现少量的As，就足以对人体的健康发生危害。长期饮用含As的水，将可能导致皮肤色素沉积、皮肤角质化、皮肤癌、膀胱癌、高血压、心脑血管病、神经病变、糖尿病等一系列健康问题。鉴于As对人体健康的巨大危害以及As污染的日趋严重，1993年，WHO率先将饮用水中As的指标值由50μm/L降至10μm/L。随后，日本、欧盟、美国也分别将各自的饮用水As标准定为10μg/L。我国目前使用的《生活饮用水卫生标准》(GB5749-2006)要求饮用水中As的最大浓度必须低于10μg/L。因此对于含有高浓度砷工业废水的处理是十分紧迫的。 According to the research of the World Health Organization, as long as there is a small amount of As in drinking water, it is enough to cause harm to human health. Drinking water containing As for a long time may lead to a series of health problems such as skin pigmentation, skin keratinization, skin cancer, bladder cancer, high blood pressure, cardiovascular and cerebrovascular diseases, neuropathy, and diabetes. In view of the great harm of As to human health and the increasing pollution of As, in 1993, WHO took the lead in reducing the index value of As in drinking water from 50 μm/L to 10 μm/L. Subsequently, Japan, the European Union, and the United States also set their drinking water As standards at 10 μg/L. The "Drinking Water Hygienic Standard" (GB5749-2006) currently used in my country requires that the maximum concentration of As in drinking water must be lower than 10 μg/L. Therefore, the treatment of industrial wastewater containing high concentration of arsenic is very urgent.
目前，混凝除As法中铝、铁基絮凝剂被广泛应用，该方法主要是利用混凝剂强大的吸附作用吸附砷，然后通过过滤或用滤膜除去水中的砷。实验结果表明，铁盐对砷的去除效率明显高于铝盐。铁盐是最经济、最有效的沉淀剂。但是As(III)毒性较大且难以被絮凝实现完全的去除。而As(V)的毒性相对较小，并且易被吸附，得以高效去除。因此应用絮凝技术除砷之前需要对 As(III)进行预氧化，即把AS(III)先氧化成As(V)，然后再进行去除。常用的氧化剂主要有漂白粉、双氧水、氯气、臭氧和二氧化锰等。但该方法需要投加大量的絮凝剂，产生大量的含砷废渣也会造成二次污染，因此使该方法的应用受到限制。 At present, aluminum and iron-based flocculants are widely used in coagulation removal of As. This method mainly uses the strong adsorption of coagulant to adsorb arsenic, and then removes arsenic in water by filtration or filter membrane. The experimental results showed that the removal efficiency of arsenic by iron salt was significantly higher than that by aluminum salt. Iron salt is the most economical and effective precipitant. However, As(III) is highly toxic and difficult to be completely removed by flocculation. However, As(V) is relatively less toxic and is easily adsorbed, so it can be removed efficiently. Therefore, it is necessary to pre-oxidize As(III) before applying flocculation technology to remove arsenic, that is, to oxidize AS(III) to As(V) first, and then remove it. Commonly used oxidants mainly include bleaching powder, hydrogen peroxide, chlorine, ozone and manganese dioxide. However, this method needs to add a large amount of flocculant, and a large amount of arsenic-containing waste residue will also cause secondary pollution, so the application of this method is limited.
目前，在进行广泛研究的是光催化技术，利用紫外光激发光催化剂（如二氧化钛）产生活性物质羟基自由基，以此来实现对三价砷的氧化。但是催化剂价格成本高、难回收、易产生污泥等缺点极大的限制了其工业应用。同时，先未有利用紫外光激发草酸氧化水体中三价砷的处理方法的相关报道。 At present, extensive research is being carried out on photocatalytic technology, which uses ultraviolet light to excite photocatalysts (such as titanium dioxide) to generate active species hydroxyl radicals, so as to realize the oxidation of trivalent arsenic. However, the disadvantages of catalysts, such as high price and cost, difficulty in recycling, and easy generation of sludge, greatly limit its industrial application. At the same time, there is no related report on the treatment method of using ultraviolet light to stimulate oxalic acid to oxidize trivalent arsenic in water.
发明内容 Contents of the invention
本发明针对已有的关于三价砷处理技术的缺陷，开发出一种绿色、高效的三价砷处理方法，实现对水体中三价砷As (III)的氧化，一方面有利于水体中砷的最终去除，同时水体中草酸转化为二氧化碳，实现水体的清洁。 Aiming at the defects of the existing trivalent arsenic treatment technology, the present invention develops a green and efficient trivalent arsenic treatment method to realize the oxidation of trivalent arsenic As(III) in the water body, which is beneficial to the arsenic in the water body on the one hand. At the same time, the oxalic acid in the water body is converted into carbon dioxide to realize the cleanliness of the water body.
本发明的技术方案是： Technical scheme of the present invention is:
一种利用紫外光激发草酸氧化水体中三价砷的处理方法，所述处理方法包括：将待处理的含有三价砷As(III)的水体中加入草酸，调节pH值，在紫外光激发下将水体中As(III)氧化为As(V)，同时水体中草酸转化为二氧化碳。 A treatment method for using ultraviolet light to excite oxalic acid to oxidize trivalent arsenic in water, the treatment method comprising: adding oxalic acid to the water body containing trivalent arsenic As(III) to be treated, adjusting the pH value, and under the excitation of ultraviolet light Oxidize As(III) in water to As(V), and convert oxalic acid in water to carbon dioxide.
优选的，草酸/As(III)的摩尔比不小于1。 Preferably, the molar ratio of oxalic acid/As(III) is not less than 1.
优选的，草酸/As(III)的摩尔比1～10：1 Preferably, the molar ratio of oxalic acid/As(III) is 1-10:1
优选的，采用硫酸或盐酸调节pH值调节至2-6。 Preferably, sulfuric acid or hydrochloric acid is used to adjust the pH value to 2-6.
优选的，所述紫外光的强度为175-400W，并根据处理要求选择光照时间一般为30-120min。 Preferably, the intensity of the ultraviolet light is 175-400W, and the illumination time is generally 30-120min according to the processing requirements.
自然界水体中含有大量的有机酸，这些有机酸主要来自于植被体液以及有机生物降解的中间产物或者最终产物，例如草酸即是一种水体中常见的有机酸，其浓度可达到20mM。但是这些有机物可通过直接或间接的方式，影响水体物理、化学和生物性质。存在于水体中的这些有机物在发生生物降解过程中会耗用水体中的溶解氧，当氧化降解过程中消耗的氧不能及时补充时，将导致水中溶解氧迅速降低，同时这些有机物将进行厌氧分解，产生有机酸、醇、醛类物质以及其它还原性产物，使水体缺氧，变黑发臭，水质恶化，导致鱼类以及水生生物缺氧窒息或中毒死亡，造成水体的富营养化，使水体的可利用性大大降低。 Natural water contains a large amount of organic acids, which mainly come from vegetation body fluids and intermediate or final products of organic biodegradation. For example, oxalic acid is a common organic acid in water, and its concentration can reach 20mM. However, these organic substances can affect the physical, chemical and biological properties of water bodies through direct or indirect ways. These organic substances in the water body will consume dissolved oxygen in the water body during the biodegradation process. When the oxygen consumed in the oxidative degradation process cannot be replenished in time, the dissolved oxygen in the water will decrease rapidly, and these organic substances will undergo anaerobic degradation. Decompose, produce organic acids, alcohols, aldehydes and other reducing products, make the water body hypoxic, turn black and smelly, deteriorate the water quality, lead to suffocation or poisoning of fish and aquatic organisms, and cause eutrophication of the water body. The availability of water bodies is greatly reduced. the
而本发明利用了水体中存在的草酸，在紫外光的激发下实现对具有剧毒性物质三价砷的氧化处理，最终三价砷转化为毒性更小、更易通过物理技术脱除、固定的五价砷。同时水体中的草酸转化为二氧化碳，实现水体的有机物的去除。因此该技术方案为水体中砷的氧化提供了一种高效、清洁的处理思路。 However, the present invention utilizes the oxalic acid present in the water body to oxidize the highly toxic trivalent arsenic under the excitation of ultraviolet light, and finally the trivalent arsenic is transformed into less toxic and easier to remove and fix by physical technology. pentavalent arsenic. At the same time, the oxalic acid in the water body is converted into carbon dioxide to realize the removal of organic matter in the water body. Therefore, this technical solution provides an efficient and clean treatment idea for the oxidation of arsenic in water.
氧化原理：草酸在紫外光的作用下，结构发生变化，生成三重态有机物，在分子氧存在的情况下能够产生羟基自由基、单线氧、超氧自由基等活性物质，进而可以氧化三价砷。 Oxidation principle: Under the action of ultraviolet light, the structure of oxalic acid changes to form triplet organic compounds. In the presence of molecular oxygen, it can produce active substances such as hydroxyl radicals, singlet oxygen, and superoxide radicals, which can then oxidize trivalent arsenic. .
与现有技术相比，本发明的有益效果是： Compared with the prior art, the beneficial effects of the present invention are:
（1）利用水体中常见的小分子有机酸草酸为反应物，在紫外光源激发下即可实现将水体中剧毒性三价砷转化为毒性更小、更易去除的五价砷，成本低，高效，环保。 (1) Using oxalic acid, a small molecule organic acid commonly found in water bodies, as a reactant, the highly toxic trivalent arsenic in water can be converted into pentavalent arsenic, which is less toxic and easier to remove, under the excitation of ultraviolet light sources, and the cost is low. Efficient and environmentally friendly.
（2）本发明的处理方法在氧化三价砷的同时还可以同时将水体中有机酸转化为二氧化碳，实现水体的自清洁，该技术绿色环保，无危害，可大范围使用。 (2) The treatment method of the present invention can simultaneously convert organic acids in the water body into carbon dioxide while oxidizing trivalent arsenic, so as to realize the self-cleaning of the water body. This technology is green, environmentally friendly, harmless, and can be widely used.
附图说明 Description of drawings
图1为本发明实施例1在紫外光激发下As(III)的氧化效率 Fig. 1 is the oxidation efficiency of As(III) under the excitation of ultraviolet light in Example 1 of the present invention
图2为本发明实施例2在紫外光激发下As(III)的氧化效率 Fig. 2 is the oxidation efficiency of As(III) under the excitation of ultraviolet light in Example 2 of the present invention
图3为本发明实施例3在紫外光激发下As(III)的氧化效率 Fig. 3 is the oxidation efficiency of As(III) under the excitation of ultraviolet light in Example 3 of the present invention
图4为本发明实施例4在紫外光激发下As(III)的氧化效率 Figure 4 is the oxidation efficiency of As(III) under the excitation of ultraviolet light in Example 4 of the present invention
图5为本发明实施例5在紫外光激发下As(III)的氧化效率。 Fig. 5 is the oxidation efficiency of As(III) under the excitation of ultraviolet light in Example 5 of the present invention.
具体实施方式 Detailed ways
下面结合附图说明本发明的具体实施方式： The specific embodiment of the present invention is described below in conjunction with accompanying drawing:
实施例1： Example 1:
As(III)浓度为0.1mM、草酸浓度为0.5mM的混合溶液500mL，并用硫酸将pH值调至4，分别注入上海比朗公司BL-GHX-I型光催化反应器中，工作时紫外光强度为400W，处理时间为50min。 As(III) concentration is 0.1mM, oxalic acid concentration is 0.5mM mixed solution 500mL, and the pH value is adjusted to 4 with sulfuric acid, respectively injected into the BL-GHX-I type photocatalytic reactor of Shanghai Bilang Company, and the ultraviolet light The intensity is 400W, and the processing time is 50min.
如图1所示，在处理过程中废水溶液中的五价砷含量不断的增加，而未添加草酸时，三价砷只能发生缓慢的氧化，其主要原因是溶解氧的作用。 As shown in Figure 1, the content of pentavalent arsenic in the wastewater solution increases continuously during the treatment process, but when no oxalic acid is added, trivalent arsenic can only be oxidized slowly, mainly due to the effect of dissolved oxygen.
实施例2： Example 2:
As(III)浓度为0.1mM、草酸浓度为0.3mM混合，用硫酸将pH值调至2，紫外光强度为400W，处理时间为40min。 The concentration of As(III) was 0.1 mM and the concentration of oxalic acid was 0.3 mM, and the pH value was adjusted to 2 with sulfuric acid, the intensity of ultraviolet light was 400 W, and the treatment time was 40 min.
如图2所示，发现：草酸量越大，pH越小三价砷的氧化效果更好 As shown in Figure 2, it is found that the greater the amount of oxalic acid, the lower the pH and the better the oxidation effect of trivalent arsenic
实施例3： Example 3:
As(III)浓度为0.1mM、草酸浓度为1mM混合，用硫酸将pH值调至6，紫外光强度为400W，处理时间为100min。 The concentration of As(III) was 0.1 mM and the concentration of oxalic acid was 1 mM, and the pH value was adjusted to 6 with sulfuric acid, the intensity of ultraviolet light was 400 W, and the treatment time was 100 min.
如图3所示，发现：草酸量增大，但是pH较大时，三价砷的氧化速率变慢。 As shown in FIG. 3 , it was found that the oxidation rate of trivalent arsenic became slower when the amount of oxalic acid was increased but the pH was higher.
实施例4： Example 4:
As(III)浓度为0.1mM、草酸浓度为0.1mM混合，用硫酸将pH值调至4，紫外光强度为400W，处理时间为60min。 The concentration of As(III) was 0.1 mM, the concentration of oxalic acid was 0.1 mM and mixed, the pH value was adjusted to 4 with sulfuric acid, the intensity of ultraviolet light was 400 W, and the treatment time was 60 min.
如图4所示，发现：当As(III)/草酸为1:1时，三价砷依然可以完全得以氧化。 As shown in Figure 4, it was found that when the As(III)/oxalic acid ratio was 1:1, trivalent arsenic could still be completely oxidized.
实施例5： Example 5:
As(III)浓度为0.1mM、草酸浓度为0.1mM混合，用硫酸将pH值调至4，紫外光强度为175W，处理时间为120min。 The concentration of As(III) was 0.1 mM, the concentration of oxalic acid was 0.1 mM and mixed, the pH value was adjusted to 4 with sulfuric acid, the intensity of ultraviolet light was 175 W, and the treatment time was 120 min.
如图5所示，发现：当As(III)/草酸为1:1时，在紫外光强度为175W时三价砷在120min内即可得以完全氧化。 As shown in Figure 5, it was found that when As(III)/oxalic acid ratio was 1:1, trivalent arsenic could be completely oxidized within 120 min when the UV light intensity was 175W.
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