CN103657593B - A kind of method of sunflower seed shell biomass carbon adsorbent, preparation method and removal water Methylene Blue - Google Patents
A kind of method of sunflower seed shell biomass carbon adsorbent, preparation method and removal water Methylene Blue Download PDFInfo
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- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 229960000907 methylthioninium chloride Drugs 0.000 title claims abstract description 50
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 15
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
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Abstract
一种葵花籽壳生物质炭吸附剂、制备方法及去除水中亚甲基蓝的方法,属于废水处理技术领域,水清洗葵花籽壳,干燥,破碎、筛分至300~600μm,再将葵花籽壳颗粒与氯化锌溶液混合浸渍,微波处理,所得葵花籽壳生物质炭经酸洗、水洗、干燥,即得到葵花籽壳生物质炭吸附剂。所得吸附剂用于去除废水中亚甲基蓝的方法,本发明方法操作简单,成本低,高效环保。A sunflower seed shell biochar adsorbent, preparation method and method for removing methylene blue in water belong to the technical field of wastewater treatment. The sunflower seed shell is washed with water, dried, crushed and sieved to 300-600 μm, and then the sunflower seed shell particles are mixed with the The zinc chloride solution is mixed and impregnated, treated with microwaves, and the obtained sunflower seed shell biochar is pickled, washed with water and dried to obtain the sunflower seed shell biochar adsorbent. The obtained adsorbent is used in a method for removing methylene blue in waste water. The method of the invention has simple operation, low cost, high efficiency and environmental protection.
Description
技术领域technical field
本发明属于废水处理技术领域,涉及一种利用吸附剂去除废水中亚甲基蓝的方法,特别是涉及一种利用葵花籽壳生物质炭吸附剂去除废水中亚甲基蓝的方法。The invention belongs to the technical field of wastewater treatment, and relates to a method for removing methylene blue in wastewater by using an adsorbent, in particular to a method for removing methylene blue in wastewater by using a sunflower seed shell biomass carbon adsorbent.
背景技术Background technique
亚甲基蓝是一种芳香杂环化合物,属于吩噻嗪类碱性染料,常用于麻、蚕丝织物、纸张的染色和竹、木的着色,可用于制造墨水和生物、细菌组织的染色等方面,还可用作化学指示剂和药物。急性摄入大量的亚甲基蓝会引起心率增加、呕吐、休克及四肢麻痹等。除此之外,高剂量的亚甲基蓝还会导致亨氏小体贫血或其他红细胞形态改变的症状,降低红细胞寿命。Methylene blue is an aromatic heterocyclic compound, which belongs to phenothiazine basic dyes. It is often used in the dyeing of hemp, silk fabrics, paper, and bamboo and wood. It can be used in the manufacture of ink and the dyeing of biological and bacterial tissues. Can be used as chemical indicator and medicine. Acute ingestion of large amounts of methylene blue can cause increased heart rate, vomiting, shock, and paralysis of limbs. In addition, high doses of methylene blue can also cause Heinz body anemia or other symptoms of red blood cell morphology changes and reduce the lifespan of red blood cells.
生物质炭,是指由富含碳的生物质通过裂解或者不完全燃烧生成的一种生物质。生物质炭具有较大的比表面积,而且表面含有较多的含氧活性官能团,可以用于吸附污水或土壤中的有机污染物和重金属,同时因其成本低廉,被认为是一种有广阔应用前景的吸附材料。用农林废弃物、工业废弃物等含碳有机废物制备生物质炭不仅可以减少固体废弃物的环境污染,还可以有效实现这些有机废物的资源化。Biochar refers to a kind of biomass produced by pyrolysis or incomplete combustion of carbon-rich biomass. Biochar has a large specific surface area, and the surface contains more oxygen-containing active functional groups, which can be used to adsorb organic pollutants and heavy metals in sewage or soil. At the same time, because of its low cost, it is considered to be a widely used Adsorbent material in the foreground. The preparation of biochar from carbon-containing organic wastes such as agricultural and forestry wastes and industrial wastes can not only reduce the environmental pollution of solid wastes, but also effectively realize the resource utilization of these organic wastes.
葵花籽是世界五大油料作物之一。中国是葵花籽的生产大国,2011年产量为231.3万吨。目前葵花籽最广泛的用途是作为一种炒制品销售,也是一种最传统的用途。随着科技的进步和食品工业的发展,人们不断开发葵花籽新的食用及经济价值,例如利用葵花籽仁榨油和制作保健品饮料、酸乳等产品,葵花籽饼粕可用作饲料等。然而,一直以来对葵花籽壳的利用比较少,除做燃料外,大多直接将其当作废弃物扔掉。葵花籽含壳率一般为22~40%,以2011年为例,葵花籽壳的年产量为50.9~92.5万吨。如果利用其制备吸附剂,不仅可以变废为宝,而且能够减轻葵花籽壳造成的污染,同时实现了葵花籽壳的资源化和经济价值。利用葵花籽壳生物炭吸附剂处理废水中的亚甲基蓝,可以有效地去除废水中的亚甲基蓝,还达到了以废治废的效果。Sunflower seed is one of the five largest oil crops in the world. China is a major producer of sunflower seeds, with an output of 2.313 million tons in 2011. The most widely used use of sunflower seeds is sold as a stir-fry product, which is also one of the most traditional uses. With the advancement of science and technology and the development of the food industry, people continue to develop new edible and economic values of sunflower seeds, such as using sunflower seeds to extract oil and make health drinks, yogurt and other products, sunflower seed cakes can be used as feed, etc. . However, the utilization of sunflower seed husks has been relatively seldom, and most of them are directly thrown away as waste except as fuel. The shell content of sunflower seeds is generally 22-40%. Taking 2011 as an example, the annual output of sunflower seed shells was 509,000-925,000 tons. If it is used to prepare an adsorbent, it can not only turn waste into treasure, but also reduce the pollution caused by sunflower seed husks, and at the same time realize the resource utilization and economic value of sunflower seed husks. Using sunflower seed shell biochar adsorbent to treat methylene blue in wastewater can effectively remove methylene blue in wastewater, and also achieve the effect of treating waste with waste.
发明内容Contents of the invention
本发明所要解决的第一个技术问题在于提供一种高效、低成本的去除废水中亚甲基蓝的吸附剂。The first technical problem to be solved by the present invention is to provide an efficient and low-cost adsorbent for removing methylene blue in wastewater.
本发明所要解决的第二个技术问题在于提供一种高效、低成本的去除废水中亚甲基蓝的方法。The second technical problem to be solved by the present invention is to provide an efficient and low-cost method for removing methylene blue in wastewater.
一种葵花籽壳生物质炭吸附剂,为微波处理的葵花籽壳作为吸附剂。The invention discloses a sunflower seed hull biochar adsorbent, which uses microwave-treated sunflower seed hulls as the adsorbent.
上述葵花籽壳生物质炭吸附剂的制备方法包括以下步骤:The preparation method of above-mentioned sunflower seed shell biochar adsorbent comprises the following steps:
用自来水清洗葵花籽壳,干燥,破碎、筛分至300~600μm,再将葵花籽壳颗粒与氯化锌溶液混合浸渍,微波处理,用盐酸溶液酸洗所得葵花籽壳生物质炭,再用蒸馏水清洗至pH呈中性,干燥,即得到葵花籽壳生物质炭吸附剂。Wash the sunflower seed shells with tap water, dry, crush, and sieve to 300-600 μm, then mix and impregnate the sunflower seed shell particles with zinc chloride solution, microwave treatment, pickle the obtained sunflower seed shell biochar with hydrochloric acid solution, and use Wash with distilled water until the pH is neutral, and dry to obtain the sunflower seed shell biochar adsorbent.
上述氯化锌溶液的浓度优选55%~75%,葵花籽壳颗粒与氯化锌溶液的浸渍比优选葵花籽壳颗粒(g):氯化锌溶液(g)为1:5~1:7,微波功率优选480~640W,微波处理时间优选10~15min,盐酸溶液的浓度优选10%。The concentration of the above-mentioned zinc chloride solution is preferably 55% to 75%, and the impregnation ratio of sunflower seed hull particles to zinc chloride solution is preferably 1:5 to 1:7 for sunflower seed hull particles (g): zinc chloride solution (g) , The microwave power is preferably 480-640W, the microwave treatment time is preferably 10-15min, and the concentration of the hydrochloric acid solution is preferably 10%.
上述所述葵花籽壳生物质炭吸附剂用于去除废水中亚甲基蓝的方法,包括以下步骤:The method that the above-mentioned sunflower seed shell biochar adsorbent is used for removing methylene blue in waste water may further comprise the steps:
在含亚甲基蓝的溶液中加入葵花籽壳生物质炭吸附剂和氯化钠,在20~60℃下吸附2~24h后,过滤分离,滤液调至中性后排放。Add sunflower seed shell biochar adsorbent and sodium chloride to the solution containing methylene blue, adsorb at 20-60°C for 2-24 hours, filter and separate, adjust the filtrate to neutrality, and then discharge.
优选含亚甲基蓝的溶液中亚甲基蓝的浓度100~900mg/L、溶液pH为2~12,葵花籽壳生物质炭吸附剂用量为2~5g/L,氯化钠的质量百分比浓度不超过30%。Preferably, the concentration of methylene blue in the solution containing methylene blue is 100-900 mg/L, the pH of the solution is 2-12, the amount of sunflower seed shell biochar adsorbent is 2-5 g/L, and the mass percentage concentration of sodium chloride is not more than 30%.
与现有技术相比,本发明的优点在于:与离子交换、膜分离、沉淀等方法相比,本发明的去除废水中亚甲基蓝的方法操作简单,成本低,高效环保。本发明所述的葵花籽壳生物质炭吸附剂吸附量大,亚甲基蓝吸附值为384.64mg/g,远超过木质净水用活性炭国家标准(135mg/g,中华人民共和国国家标准GB13803.2-1999),同时开辟了葵花籽壳资源化利用的新途径。Compared with the prior art, the present invention has the advantages that: compared with methods such as ion exchange, membrane separation, and precipitation, the method for removing methylene blue in wastewater is simple to operate, low in cost, highly efficient and environmentally friendly. The sunflower seed shell biomass carbon adsorbent of the present invention has a large adsorption capacity, and the methylene blue adsorption value is 384.64 mg/g, far exceeding the national standard (135 mg/g, National Standard GB13803.2-1999 of the People's Republic of China for activated carbon for wood water purification) ), and at the same time opened up a new way of resource utilization of sunflower seed hulls.
附图说明Description of drawings
图1为pH对亚甲基蓝去除效果的影响。Figure 1 is the effect of pH on the removal effect of methylene blue.
图2为亚甲基蓝初始浓度对亚甲基蓝去除效果的影响。Figure 2 is the effect of the initial concentration of methylene blue on the removal effect of methylene blue.
图3为氯化钠浓度对亚甲基蓝去除效果的影响。Fig. 3 is the influence of sodium chloride concentration on methylene blue removal effect.
图4为Langmuir吸附等温线。Figure 4 shows the Langmuir adsorption isotherm.
图5为本发明的葵花籽壳生物质炭吸附剂的红外光谱图。Fig. 5 is the infrared spectrogram of the sunflower seed shell biochar adsorbent of the present invention.
具体实施方式Detailed ways
下面结合具体实施例来对本发明作进一步详细说明,但本发明并不限制于实施例。The present invention will be described in further detail below in conjunction with specific examples, but the present invention is not limited to the examples.
实施例1Example 1
取一定质量的葵花籽壳,自来水冲洗数次,干燥,破碎、筛分至300~600μm,将葵花籽壳颗粒与氯化锌溶液按照葵花籽壳颗粒质量(g):氯化锌溶液质量(g)为1:7的比例混合浸渍于锥形瓶中,其中氯化锌溶液的浓度为55%。480W微波处理15min后,用浓度为10%的盐酸溶液酸洗所得葵花籽壳生物质炭,再用蒸馏水清洗至pH呈中性,干燥,即得到葵花籽壳生物质炭吸附剂。Take a certain quality of sunflower seed shells, rinse them with tap water for several times, dry, crush, and sieve to 300-600 μm, mix the sunflower seed shell particles and zinc chloride solution according to the mass of sunflower seed shell particles (g): the mass of zinc chloride solution ( g) Mix and impregnate in a conical flask at a ratio of 1:7, in which the concentration of zinc chloride solution is 55%. After 480W microwave treatment for 15 minutes, the obtained sunflower seed shell biochar was pickled with 10% hydrochloric acid solution, then washed with distilled water until the pH was neutral, and dried to obtain the sunflower seed shell biochar adsorbent.
取0.1g本实施例制备的吸附剂和5g氯化钠加入溶液pH值分别为2、4、6、7、8、10、12,50mL,100mg/L的亚甲基蓝溶液中,于20℃下恒温水浴摇床中振荡2h后,过滤分离,滤液调至中性后排放。Take 0.1 g of the adsorbent prepared in this example and 5 g of sodium chloride and add it into the methylene blue solution with pH values of 2, 4, 6, 7, 8, 10, 12, 50 mL and 100 mg/L respectively, and keep the temperature at 20 ° C After shaking in a water-bath shaker for 2 hours, filter and separate, and discharge the filtrate after adjusting to neutrality.
不同初始pH对亚甲基蓝去除效果的影响如图1所示,可以看出pH对亚甲基蓝吸附值的影响很小,说明本发明的去除亚甲基蓝的方法基本不受pH限制。The influence of different initial pH on the methylene blue removal effect is as shown in Figure 1, and it can be seen that the influence of pH on the methylene blue adsorption value is very small, illustrating that the method for removing methylene blue of the present invention is not limited by pH substantially.
实施例2Example 2
取一定质量的葵花籽壳,自来水冲洗数次,干燥,破碎、筛分至300~600μm,将葵花籽壳颗粒与氯化锌溶液按照葵花籽壳颗粒质量(g):氯化锌溶液质量(g)为1:6.5的比例混合浸渍于锥形瓶中,其中氯化锌溶液的浓度为60%。520W微波处理14min后,用浓度为10%的盐酸溶液酸洗所得葵花籽壳生物质炭,再用蒸馏水清洗至pH呈中性,干燥,即得到葵花籽壳生物质炭吸附剂。Take a certain quality of sunflower seed shells, rinse them with tap water for several times, dry, crush, and sieve to 300-600 μm, mix the sunflower seed shell particles and zinc chloride solution according to the mass of sunflower seed shell particles (g): the mass of zinc chloride solution ( g) Mix and impregnate in a conical flask at a ratio of 1:6.5, in which the concentration of zinc chloride solution is 60%. After 14 minutes of microwave treatment at 520W, the obtained sunflower seed shell biochar was pickled with a 10% hydrochloric acid solution, washed with distilled water until the pH was neutral, and dried to obtain the sunflower seed shell biochar adsorbent.
取0.15g本实施例制备的吸附剂和2.5g氯化钠加入分别含100、300、500、700、900mg/L亚甲基蓝的50mL溶液中,于20℃下恒温水浴摇床中振荡24h后,过滤分离,滤液调至中性后排放。Add 0.15 g of the adsorbent prepared in this example and 2.5 g of sodium chloride into 50 mL solutions containing 100, 300, 500, 700, and 900 mg/L methylene blue respectively, vibrate in a constant temperature water bath shaker at 20 ° C for 24 h, and filter Separation, the filtrate is adjusted to neutrality and discharged.
亚甲基蓝初始浓度对亚甲基蓝去除效果的影响如图2所示。在浓度梯度的驱动下,随着亚甲基蓝初始浓度由100mg/L增加到700mg/L,亚甲基蓝吸附值由51.21mg/g上升到343.27mg/g,而去除率仅由99.82%下降到97.60%。亚甲基蓝初始浓度为900mg/L时亚甲基蓝吸附值为392.80mg/g,去除率为87.45%。这表明本发明的去除亚甲基蓝的方法适用于含100~700mg/L亚甲基蓝的废水处理。The effect of the initial concentration of methylene blue on the removal effect of methylene blue is shown in Figure 2. Driven by the concentration gradient, as the initial concentration of methylene blue increased from 100 mg/L to 700 mg/L, the adsorption value of methylene blue increased from 51.21 mg/g to 343.27 mg/g, while the removal rate only decreased from 99.82% to 97.60%. When the initial concentration of methylene blue was 900mg/L, the adsorption value of methylene blue was 392.80mg/g, and the removal rate was 87.45%. This shows that the method for removing methylene blue of the present invention is suitable for the treatment of wastewater containing 100-700 mg/L methylene blue.
实施例3Example 3
取一定质量的葵花籽壳,自来水冲洗数次,干燥,破碎、筛分至300~600μm,将葵花籽壳颗粒与氯化锌溶液按照葵花籽壳颗粒质量(g):氯化锌溶液质量(g)为1:6的比例混合浸渍于锥形瓶中,其中氯化锌溶液的浓度为65%。560W微波处理13min后,用浓度为10%的盐酸溶液酸洗所得葵花籽壳生物质炭,再用蒸馏水清洗至pH呈中性,干燥,即得到葵花籽壳生物质炭吸附剂。Take a certain quality of sunflower seed shells, rinse them with tap water for several times, dry, crush, and sieve to 300-600 μm, mix the sunflower seed shell particles and zinc chloride solution according to the mass of sunflower seed shell particles (g): the mass of zinc chloride solution ( g) Mix and impregnate in a conical flask in a ratio of 1:6, in which the concentration of zinc chloride solution is 65%. After 560W microwave treatment for 13 minutes, the obtained sunflower seed shell biochar was pickled with 10% hydrochloric acid solution, then washed with distilled water until the pH was neutral, and dried to obtain the sunflower seed shell biochar adsorbent.
取本实施例制备的吸附剂0.20g加入氯化钠使其质量百分比浓度分别为0%、2%、5%、10%、15%、30%,50mL、100mg/L的亚甲基蓝溶液中,于20℃下恒温水浴摇床中振荡2h后,过滤分离,滤液调至中性后排放。Take 0.20 g of the adsorbent prepared in this example and add sodium chloride to make the mass percent concentration respectively 0%, 2%, 5%, 10%, 15%, 30%, 50mL, 100mg/L methylene blue solution, in Shake in a constant temperature water-bath shaker at 20°C for 2 hours, then filter and separate, and discharge the filtrate after adjusting it to neutral.
氯化钠浓度对亚甲基蓝去除效果的影响如图3所示。氯化钠浓度较高时(15%和30%)吸附速率较快,但是不同氯化钠浓度对吸附量的影响不显著,葵花籽壳生物质炭吸附剂可以在比较宽的氯化钠浓度范围内(0%~30%)实现对亚甲基蓝的吸附去除。The effect of sodium chloride concentration on the removal effect of methylene blue is shown in Figure 3. When the concentration of sodium chloride is higher (15% and 30%), the adsorption rate is faster, but the effect of different sodium chloride concentrations on the adsorption capacity is not significant. Within the range (0% to 30%), the adsorption and removal of methylene blue can be realized.
实施例4Example 4
取一定质量的葵花籽壳,自来水冲洗数次,干燥,破碎、筛分至300~600μm,将葵花籽壳颗粒与氯化锌溶液按照葵花籽壳颗粒质量(g):氯化锌溶液质量(g)为1:5.5的比例混合浸渍于锥形瓶中,其中氯化锌溶液的浓度为70%。600W微波处理12min后,用浓度为10%的盐酸溶液酸洗所得葵花籽壳生物质炭,再用蒸馏水清洗至pH呈中性,干燥,即得到葵花籽壳生物质炭吸附剂。Take a certain quality of sunflower seed shells, rinse them with tap water for several times, dry, crush, and sieve to 300-600 μm, mix the sunflower seed shell particles and zinc chloride solution according to the mass of sunflower seed shell particles (g): the mass of zinc chloride solution ( g) Mix and impregnate in a conical flask at a ratio of 1:5.5, in which the concentration of zinc chloride solution is 70%. After 600W microwave treatment for 12 minutes, the obtained sunflower seed shell biochar was pickled with 10% hydrochloric acid solution, then washed with distilled water until the pH was neutral, and dried to obtain the sunflower seed shell biochar adsorbent.
取0.25g本实施例制备的吸附剂和2.5g氯化钠加入到50mL分别含100,300,500,700,900mg/L亚甲基蓝的溶液中,于20℃,40℃,60℃下恒温水浴摇床中振荡21h后,过滤分离,滤液调至中性后排放。Add 0.25 g of the adsorbent prepared in this example and 2.5 g of sodium chloride into 50 mL of solutions containing 100, 300, 500, 700, and 900 mg/L methylene blue respectively, shake in a constant temperature water bath at 20°C, 40°C, and 60°C After oscillating in the bed for 21 hours, filter and separate, and adjust the filtrate to neutrality before discharging.
吸附结果用Langmuir吸附等温线拟合,不同温度下的吸附等温线如图4所示,拟合结果如表1所示。The adsorption results were fitted by Langmuir adsorption isotherms. The adsorption isotherms at different temperatures are shown in Fig. 4, and the fitting results are shown in Table 1.
从图4和表1可以看出,Langmuir模型对葵花籽壳生物质炭吸附剂对亚甲基蓝的等温吸附试验数据的拟合效果很好,因此Langmuir模型可以很好地描述葵花籽壳生物质炭吸附剂对亚甲基蓝的等温吸附试验数据。从表1可以看出,Q0和b均随着温度的升高而下降,这表明葵花籽壳生物质炭吸附剂的表面活性随着温度的升高而下降,与亚甲基蓝分子在低温条件下有更高的亲和性,即葵花壳生物质炭吸附剂在低温条件下对亚甲基蓝的吸附效果更好。表明本发明的工艺流程对操作条件及设备要求低,是一种经济、节约能源的含亚甲基蓝废水处理方法,适于推广与应用。It can be seen from Figure 4 and Table 1 that the Langmuir model fits the isothermal adsorption test data of sunflower seed shell biochar adsorbent to methylene blue very well, so the Langmuir model can well describe the adsorption of sunflower seed shell biomass charcoal The isothermal adsorption test data of the solvent on methylene blue. It can be seen from Table 1 that both Q0 and b decrease with the increase of temperature, which indicates that the surface activity of sunflower seed shell biochar adsorbent decreases with the increase of temperature, and has the same effect with methylene blue molecules at low temperature. Higher affinity, that is, the sunflower shell biochar adsorbent has a better adsorption effect on methylene blue at low temperature. It shows that the technological process of the present invention has low requirements on operating conditions and equipment, is an economical and energy-saving treatment method for wastewater containing methylene blue, and is suitable for popularization and application.
20℃时,用Langmuir等温线计算得到的葵花籽壳生物质炭吸附剂吸附亚甲基蓝的最大单分子层吸附量Q0是384.62mg/g,远超过木质净水用活性炭国家标准(135mg/g,中华人民共和国国家标准GB13803.2-1999),说明本发明的改性葵花籽壳可以作为处理含亚甲基蓝废水的一种高效低成本的吸附剂。At 20°C, the maximum monomolecular layer adsorption Q0 of sunflower seed shell biochar adsorbent for methylene blue calculated by Langmuir isotherm is 384.62 mg/g, far exceeding the national standard of activated carbon for wood water purification (135 mg/g, The National Standard of the People's Republic of China GB13803.2-1999), illustrates that the modified sunflower seed shell of the present invention can be used as an efficient and low-cost adsorbent for treating wastewater containing methylene blue.
表1Langmuir吸附等温线参数Table 1 Langmuir adsorption isotherm parameters
实施例5Example 5
取一定质量的葵花籽壳,自来水冲洗数次,干燥,破碎、筛分至300~600μm,将葵花籽壳颗粒与氯化锌溶液按照葵花籽壳颗粒质量(g):氯化锌溶液质量(g)为1:5的比例混合浸渍于锥形瓶中,其中氯化锌溶液的浓度为75%。640W微波处理10min后,用浓度为10%的盐酸溶液酸洗所得葵花籽壳生物质炭,再用蒸馏水清洗至pH呈中性,干燥,即得到葵花籽壳生物质炭吸附剂。Take a certain quality of sunflower seed shells, rinse them with tap water for several times, dry, crush, and sieve to 300-600 μm, mix the sunflower seed shell particles and zinc chloride solution according to the mass of sunflower seed shell particles (g): the mass of zinc chloride solution ( g) Mix and impregnate in a conical flask in a ratio of 1:5, in which the concentration of zinc chloride solution is 75%. After 640W microwave treatment for 10 minutes, the obtained sunflower seed shell biochar was pickled with 10% hydrochloric acid solution, then washed with distilled water until the pH was neutral, and dried to obtain the sunflower seed shell biochar adsorbent.
对本实施例制备的葵花籽壳生物质炭吸附剂进行红外光谱分析。Infrared spectrum analysis was carried out on the sunflower seed hull biochar adsorbent prepared in this example.
本实施例制备的葵花籽壳生物质炭吸附剂的红外光谱图如图5示。3429cm-1处的吸收峰代表羟基中O–H的伸缩振动,2924cm-1的吸收峰为脂肪族化合物中C–H与纤维素和半纤维素中CH2的伸缩振动的重叠,1694cm-1处的吸收峰由羰基中C=O的振动引起,1617cm-1处的吸收峰可能是C=O的伸缩振动,1409cm-1处的吸收峰是酯中C=O的对称伸缩振动和醇中O–H的变形振动共同作用的结果,1223cm-1处的吸收峰可能是C–N(III型胺基)伸缩振动造成的,1094cm-1处的吸收峰是膦酸基团中P–O–C和多糖类物质中C–O–C的伸缩振动的叠加,其他波段(图中指纹状附近)的吸收峰为膦酸基团或硫磺基团的振动。上述结果表明,葵花籽壳生物质炭吸附剂表面富含羟基、羰基等活性基团。The infrared spectrogram of the sunflower seed shell biochar adsorbent prepared in this example is shown in Figure 5. The absorption peak at 3429cm -1 represents the stretching vibration of O–H in hydroxyl, the absorption peak at 2924cm -1 is the overlap of C–H in aliphatic compounds and the stretching vibration of CH 2 in cellulose and hemicellulose, and the absorption peak at 1694cm -1 The absorption peak at 1617cm -1 is caused by the vibration of C=O in the carbonyl group, the absorption peak at 1617cm -1 may be the stretching vibration of C=O, the absorption peak at 1409cm -1 is the symmetric stretching vibration of C=O in the ester and the The result of the joint action of O–H deformation vibrations, the absorption peak at 1223cm -1 may be caused by the stretching vibration of C–N (type III amino group), and the absorption peak at 1094cm -1 is the P–O in the phosphonic acid group The superposition of C–O–C stretching vibrations in –C and polysaccharides, and the absorption peaks in other bands (near the fingerprints in the figure) are the vibrations of phosphonic acid groups or sulfur groups. The above results indicated that the surface of sunflower seed hull biochar adsorbent was rich in active groups such as hydroxyl and carbonyl.
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