CN112023876A - Preparation of magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material and application of phosphorus removal in wastewater - Google Patents

Preparation of magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material and application of phosphorus removal in wastewater Download PDF

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CN112023876A
CN112023876A CN202010714512.XA CN202010714512A CN112023876A CN 112023876 A CN112023876 A CN 112023876A CN 202010714512 A CN202010714512 A CN 202010714512A CN 112023876 A CN112023876 A CN 112023876A
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magnesium
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袁俊杰
王纪章
朱瑶
邱凤仙
何美莹
张涛
李萍萍
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Jiangsu University
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Abstract

本发明属于复合材料技术领域,涉及改性生物质炭材料的制备方法,具体涉及镁铝复合氧化物改性椰子壳生物质炭吸附材料的制备方法,包括:将粉碎的椰子壳浸泡在碱液中去杂,洗净,加入醋酸酸化的亚氯酸中脱色、清洗、烘干后得到椰子壳纤维;继续浸泡于硝酸铝溶液后过滤,烘干,在氮气氛围中200~800℃煅烧,得到Al2O3/CSF;按照固液比0.3~1.8 g:0.1~0.9 g:0.05~1.0 g:50~200 mL,将六水合硝酸镁、Al2O3/CSF、六亚甲基四胺溶于去离子水中,60~180℃反应6~48 h后,过滤、洗涤、高温煅烧得到Mg‑Al/CSF。本发明利用常见的废弃椰子壳作为生物质资源,通过水热、煅烧法制备而成,可实现对废水中磷的高效去除,材料可循环使用,最大程度降低制备成本,提高吸附性能。

Figure 202010714512

The invention belongs to the technical field of composite materials, and relates to a method for preparing modified biomass carbon materials, in particular to a method for preparing a magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material, comprising: soaking crushed coconut shells in lye Remove impurities, wash, add chlorous acid acidified with acetic acid to decolorize, clean and dry to obtain coconut husk fibers; continue to soak in aluminum nitrate solution, filter, dry, and calcinate at 200-800°C in nitrogen atmosphere to obtain Al 2 O 3 /CSF; according to the solid-liquid ratio of 0.3-1.8 g: 0.1-0.9 g: 0.05-1.0 g: 50-200 mL, combine magnesium nitrate hexahydrate, Al 2 O 3 /CSF, hexamethylenetetramine Dissolved in deionized water, reacted at 60-180 °C for 6-48 h, filtered, washed, and calcined at high temperature to obtain Mg-Al/CSF. The method utilizes common waste coconut shells as biomass resources, and is prepared by hydrothermal and calcining methods, which can realize the efficient removal of phosphorus in wastewater, the materials can be recycled, the preparation cost can be reduced to the greatest extent, and the adsorption performance can be improved.

Figure 202010714512

Description

镁铝复合氧化物改性椰子壳生物质炭吸附材料的制备及去除 废水中磷的应用Preparation of magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material and application of phosphorus removal in wastewater

技术领域technical field

本发明属于复合材料技术领域,涉及改性生物质炭材料的制备方法,具体涉及镁铝复合氧化物改性椰子壳生物质炭吸附材料的制备及去除废水中磷的应用。The invention belongs to the technical field of composite materials, and relates to a preparation method of modified biomass carbon materials, in particular to the preparation of magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption materials and the application of removing phosphorus in wastewater.

背景技术Background technique

近年来,随着经济发展和社会工业现代化,各种环境污染物的排放量日益增多,特别是磷排放量的急剧增加使得自然水体环境遭到严重的破坏。目前,常用的污水除磷技术有化学沉淀法、吸附法、离子交换法和生物法等。简单的沉淀法对污水中大量的磷化合物难以去除;生物法除磷处理效果有限;离子交换法存在树脂制备价格昂贵、交换容量低、选择性差等一系列缺点。吸附法具有效率高、成本低、操作简单、可再生、可持续等优点,利用吸附法除磷的关键在于吸附剂的选择。目前常用的吸附剂有活性炭、沸石等,在使用过程中往往会产生大量泥渣,应用效果较差。因此,寻找能够高效去除废水中磷的环保型吸附剂迫在眉睫。与此同时,利用生物质材料制备能作为吸附剂的复合材料在环境治理方面得到广泛关注。In recent years, with the economic development and social and industrial modernization, the discharge of various environmental pollutants is increasing, especially the sharp increase in phosphorus discharge, which has caused serious damage to the natural water environment. At present, the commonly used wastewater phosphorus removal technologies include chemical precipitation, adsorption, ion exchange and biological methods. Simple precipitation method is difficult to remove a large number of phosphorus compounds in sewage; biological phosphorus removal treatment has limited effect; ion exchange method has a series of disadvantages such as expensive resin preparation, low exchange capacity and poor selectivity. The adsorption method has the advantages of high efficiency, low cost, simple operation, regeneration, and sustainability. The key to phosphorus removal by adsorption is the selection of adsorbents. At present, the commonly used adsorbents include activated carbon, zeolite, etc., which often produce a large amount of sludge during the use process, and the application effect is poor. Therefore, it is urgent to find environmentally friendly adsorbents that can efficiently remove phosphorus from wastewater. At the same time, the use of biomass materials to prepare composite materials that can be used as adsorbents has received extensive attention in environmental governance.

以生物质为基础的炭材料通常可通过废弃农林作物得到,具有易获得、良好的吸附性能等特点而受到广泛关注,但以农林废弃物为前驱体制备用于水中磷吸附的生物质材料却很少报道。以农林废弃物作为生物质复合材料前驱体,不仅对农林废弃物进行充分利用,还能以废治废,达到保护环境的目的。生物质炭材料具有吸附能力,是去除磷的有效方法。在生物质炭材料中掺杂金属或金属氧化物能够提高吸附剂的吸附能力,且复合材料具有催化性能,可以多渠道去除污染物。Biomass-based carbon materials can usually be obtained from discarded agricultural and forestry crops, and have attracted extensive attention due to their easy availability and good adsorption properties. However, the preparation of biomass materials for phosphorus adsorption in water using agricultural and forestry wastes as precursors Report less. Using agricultural and forestry wastes as precursors of biomass composite materials can not only make full use of agricultural and forestry wastes, but also treat wastes with waste, so as to achieve the purpose of protecting the environment. Biochar material has adsorption capacity and is an effective method for phosphorus removal. Doping metal or metal oxides in the biomass carbon material can improve the adsorption capacity of the adsorbent, and the composite material has catalytic properties, which can remove pollutants through multiple channels.

本发明以废弃的椰子壳为生物质炭前驱体,选择镁铝双金属复合氧化物,通过原位生长法制备具有分级结构的镁铝双金属复合氧化物/生物质炭复合材料,并将其应用于废水中磷的去除。此外,利用农林废弃物作为吸附剂的前体,不仅使自然环境产生的废弃农林作物得到充分利用,还为去除水中磷提供了良好的吸附剂。In the invention, waste coconut shells are used as biomass carbon precursors, magnesium-aluminum bimetallic composite oxides are selected, and magnesium-aluminum bimetallic composite oxides/biomass carbon composite materials with hierarchical structure are prepared by an in-situ growth method, and the composite materials are Applied to the removal of phosphorus in wastewater. In addition, using agricultural and forestry wastes as the precursors of adsorbents not only makes full use of abandoned agricultural and forestry crops generated in the natural environment, but also provides a good adsorbent for removing phosphorus from water.

发明内容SUMMARY OF THE INVENTION

针对上述现有技术中存在的不足,本发明的目的是公开一种镁铝复合氧化物改性椰子壳生物质炭吸附材料的制备方法。In view of the above-mentioned deficiencies in the prior art, the purpose of the present invention is to disclose a preparation method of a magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material.

技术方案Technical solutions

一种镁铝复合氧化物改性椰子壳生物质炭吸附材料的制备方法,包括如下步骤:A preparation method of magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material, comprising the following steps:

a)将粉碎的椰子壳浸泡在氢氧化钠溶液中,60~150℃条件下搅拌1~8h,优选1M,80℃搅拌3h,去除杂质后,用去离子水洗净,加入醋酸酸化的亚氯酸钠溶液中进行脱色处理,然后将脱色的生物质用去离子水清洗,烘干后得到椰子壳纤维;a) Soak the crushed coconut shell in sodium hydroxide solution, stir at 60~150℃ for 1~8h, preferably 1M, stir at 80℃ for 3h, after removing impurities, wash with deionized water, add acetic acid acidified Decolorization is carried out in the sodium chlorate solution, then the decolorized biomass is washed with deionized water, and dried to obtain coconut husk fibers;

b)按照每100mL去离子水中溶解1~20g九水合硝酸铝计,将得到的椰子壳纤维浸泡5~20h后过滤,优选5g浸泡10h,烘干得到的样品在氮气氛围中200~800℃煅烧2~8h,优选400℃煅烧4h,得到氧化铝包覆的椰子壳纤维(Al2O3/CSF);b) Dissolving 1-20 g of aluminum nitrate nonahydrate per 100 mL of deionized water, soak the obtained coconut husk fibers for 5-20 h and filter, preferably soak 5 g for 10 h, and calcine the obtained sample in a nitrogen atmosphere at 200-800 °C 2~8h, preferably calcining at 400℃ for 4h, to obtain alumina-coated coconut husk fibers (Al 2 O 3 /CSF);

c)按照固液比0.3~1.8g:0.1~0.9g:0.05~1.0g:50~200mL,优选0.9g:0.3g:0.5g:75mL,将六水合硝酸镁、Al2O3/CSF、六亚甲基四胺溶于去离子水中,充分搅拌后,将混合物转移到不锈钢反应釜中,60~180℃反应6~48h后,优选120℃反应12h,过滤、洗涤,烘干后的产物在氮气氛围中200~800℃煅烧2~8h,优选500℃煅烧4h,得到镁铝复合氧化物改性椰子壳生物质炭吸附材料(Mg-Al/CSF)。c) According to the solid-liquid ratio of 0.3~1.8g:0.1~0.9g:0.05~1.0g:50~200mL, preferably 0.9g:0.3g:0.5g:75mL, mix magnesium nitrate hexahydrate, Al 2 O 3 /CSF, Hexamethylenetetramine is dissolved in deionized water, and after fully stirring, the mixture is transferred to a stainless steel reaction kettle, reacted at 60-180°C for 6-48 hours, preferably at 120°C for 12 hours, filtered, washed, and the product after drying calcined at 200-800 °C for 2-8 h in nitrogen atmosphere, preferably 500 °C for 4 h, to obtain magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material (Mg-Al/CSF).

本发明较优公开例中,所述氢氧化钠溶液浓度为0.2~1.5M,所述醋酸酸化的亚氯酸钠溶液,是将亚氯酸钠按照5%质量分数溶于水再以醋酸调节pH为4。In the preferred disclosure example of the present invention, the concentration of the sodium hydroxide solution is 0.2-1.5M, and the sodium chlorite solution acidified with acetic acid is made by dissolving sodium chlorite in water according to 5% mass fraction and adjusting it with acetic acid pH is 4.

根据本发明所述方法制得的镁铝复合氧化物改性椰子壳生物质炭吸附材料(Mg-Al/CSF),其形貌仍保留原有椰子壳纤维结构,并且表面生长的分级结构纳米片有效地提高Mg-Al/CSF材料的比表面积,从而暴露了更多的吸附位点,可用于去除废水中的磷元素。The magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material (Mg-Al/CSF) prepared according to the method of the present invention still retains the original coconut shell fiber structure in its morphology, and has a hierarchical structure nanometer grown on the surface. The flakes effectively increase the specific surface area of the Mg-Al/CSF material, thereby exposing more adsorption sites, which can be used to remove phosphorus elements in wastewater.

本发明还有一个目的,就是将所制得的镁铝复合氧化物改性椰子壳生物质炭吸附材料(Mg-Al/CSF),应用于废水除磷。Another object of the present invention is to apply the prepared magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material (Mg-Al/CSF) to phosphorus removal in wastewater.

本发明所公开的用于去除废水中的磷元素的方法,步骤如下:The method disclosed in the present invention is used to remove the phosphorus element in waste water, and the steps are as follows:

按每10mL 100mg/L的磷酸二氢钾溶液加入10~40mg Mg-Al/CSF计,调节溶液pH在3~10,温度25~45℃,吸附2h后,磷浓度用可见分光光度计在波长λ=700nm处检测,并计算得到磷的浓度。Add 10-40 mg of Mg-Al/CSF per 10 mL of 100 mg/L potassium dihydrogen phosphate solution, adjust the pH of the solution to 3-10, temperature 25-45 °C, and after adsorption for 2 hours, use a visible spectrophotometer to measure the phosphorus concentration at the wavelength of Detected at λ=700nm, and calculated the concentration of phosphorus.

磷去除率由公式(1)计算:Phosphorus removal rate is calculated by formula (1):

Figure BDA0002597669900000021
Figure BDA0002597669900000021

式中,R为去除率(%),C0(mg/L)为吸附前离子的初始浓度,Ce为吸附平衡时间为t时溶液中离子的浓度。In the formula, R is the removal rate (%), C 0 (mg/L) is the initial concentration of ions before adsorption, and C e is the concentration of ions in the solution when the adsorption equilibrium time is t.

本发明的特点为:The characteristics of the present invention are:

(1)所制得的镁铝复合氧化物改性椰子壳生物质炭吸附材料(Mg-Al/CSF)具有较好的生物相容性,且原料获取方便,制备过程简单,成本低廉;(1) The prepared magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material (Mg-Al/CSF) has good biocompatibility, and the raw materials are easily obtained, the preparation process is simple, and the cost is low;

(2)所制得的镁铝复合氧化物改性椰子壳生物质炭吸附材料(Mg-Al/CSF)具有明显的分级结构和表面较多的吸附位点,对废水中的磷有着较高的吸附容量;吸附条件温和,少量的吸附剂就能实现较高的去除率,且材料可以回收循环利用。(2) The prepared magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material (Mg-Al/CSF) has an obvious hierarchical structure and more adsorption sites on the surface, and has a higher phosphorus content in wastewater. The adsorption capacity is moderate; the adsorption conditions are mild, a small amount of adsorbent can achieve a high removal rate, and the material can be recycled and reused.

本发明所用的氢氧化钠、醋酸、盐酸、亚氯酸钠、六水合硝酸镁、六亚甲基四胺、磷酸二氢钾、九水合硝酸铝,均来自国药集团化学试剂有限公司。The sodium hydroxide, acetic acid, hydrochloric acid, sodium chlorite, magnesium nitrate hexahydrate, hexamethylenetetramine, potassium dihydrogen phosphate and aluminum nitrate nonahydrate used in the present invention all come from Sinopharm Chemical Reagent Co., Ltd.

有益效果beneficial effect

本发明公开了一种用于去除环境废水中磷元素的镁铝复合氧化物改性椰子壳生物质炭吸附材料(Mg-Al/CSF)的制备方法,利用常见的废弃椰子壳作为生物质资源,通过简单的水热、煅烧方法制备得到的复合材料,在用量很少的条件下即可实现对废水中磷的高效去除,并且材料可以循环使用,最大程度降低制备成本,提高吸附性能。该发明在高效废水除磷领域有较好的应用前景,具有节能环保和方便回收等优点。The invention discloses a preparation method of a magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material (Mg-Al/CSF) for removing phosphorus elements in environmental wastewater, and uses common waste coconut shells as biomass resources , The composite material prepared by a simple hydrothermal and calcination method can achieve efficient removal of phosphorus in wastewater under the condition of a small amount of consumption, and the material can be recycled to minimize the preparation cost and improve the adsorption performance. The invention has good application prospects in the field of high-efficiency wastewater phosphorus removal, and has the advantages of energy saving, environmental protection, convenient recovery and the like.

附图说明Description of drawings

图1.实施例3所制备的椰子壳纤维(A、B)、Al2O3/椰子壳纤维(C、D)和镁铝双金属氧化物/椰子壳炭纤维(E、F)之SEM;Fig. 1. SEM of coconut husk fibers (A, B), Al 2 O 3 /coconut husk fibers (C, D) and magnesium-aluminum bimetallic oxide/coconut husk carbon fibers (E, F) prepared in Example 3 ;

图2.实施例3所制备的CSF、Al2O3/CSF和Mg-Al/CSF之XRD。Figure 2. XRD of CSF, Al 2 O 3 /CSF and Mg-Al/CSF prepared in Example 3.

具体实施方式Detailed ways

下面结合实施例对本发明进行详细说明,以使本领域技术人员更好地理解本发明,但本发明并不局限于以下实施例。The present invention will be described in detail below in conjunction with the examples, so that those skilled in the art can better understand the present invention, but the present invention is not limited to the following examples.

除非另外限定,这里所使用的术语(包含科技术语)应当解释为具有如本发明所属技术领域的技术人员所共同理解到的相同意义。还将理解到,这里所使用的术语应当解释为具有与它们在本说明书和相关技术的内容中的意义相一致的意义,并且不应当以理想化或过度的形式解释,除非这里特意地如此限定。Unless otherwise defined, terms (including technical and scientific terms) used herein should be construed to have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will also be understood that terms used herein should be construed to have meanings consistent with their meanings in the context of this specification and related art and should not be interpreted in an idealized or excessive form unless expressly defined as such herein .

实施例1Example 1

一种镁铝复合氧化物改性椰子壳生物质炭吸附材料的制备方法,包括如下步骤:A preparation method of magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material, comprising the following steps:

a)将粉碎的椰子壳浸泡在0.2M氢氧化钠溶液中,60℃条件下搅拌1h,去除杂质后,用去离子水洗涤,加入醋酸酸化的亚氯酸钠溶液(质量分数5%)中进行脱色处理,然后将脱色的生物质用去离子水清洗,烘干后得到椰子壳纤维;a) Soak the crushed coconut shells in 0.2M sodium hydroxide solution, stir at 60°C for 1 hour, remove impurities, wash with deionized water, and add to acetic acid acidified sodium chlorite solution (mass fraction 5%) Carry out decolorization treatment, then the decolorized biomass is washed with deionized water, and the coconut husk fiber is obtained after drying;

b)按照每100mL去离子水中溶解1g九水合硝酸铝计,将得到的椰子壳纤维浸泡5h后过滤,烘干得到的样品在氮气条件下200℃煅烧2h,得到氧化铝包覆的椰子壳纤维(Al2O3/CSF);b) Dissolving 1 g of aluminum nitrate nonahydrate per 100 mL of deionized water, soak the obtained coconut husk fibers for 5 hours and then filter them. The samples obtained by drying are calcined at 200° C. for 2 hours under nitrogen conditions to obtain alumina-coated coconut husk fibers. (Al 2 O 3 /CSF);

c)按照固液比0.3g:0.1g:0.05g:50mL,将六水合硝酸镁、Al2O3/CSF、六亚甲基四胺溶于去离子水中,充分搅拌后,将混合物转移到不锈钢反应釜中,60℃反应6h后,过滤、洗涤,烘干后的产物在氮气氛围下200℃煅烧2h,得到镁铝复合氧化物改性椰子壳生物质炭吸附材料(Mg-Al/CSF)。c) According to the solid-liquid ratio of 0.3g:0.1g:0.05g:50mL, dissolve magnesium nitrate hexahydrate, Al 2 O 3 /CSF and hexamethylenetetramine in deionized water, and after thorough stirring, transfer the mixture to a In a stainless steel reactor, after reacting at 60 °C for 6 h, filtered, washed, and the dried product was calcined at 200 °C for 2 h in a nitrogen atmosphere to obtain magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material (Mg-Al/CSF ).

废水中磷的去除:Phosphorus removal from wastewater:

按每10mL 100mg/L的磷酸二氢钾溶液加入10mg Mg-Al/CSF计,调节溶液pH在3,温度25℃条件下吸附2h后,磷浓度用可见分光光度计在波长λ=700nm处检测,并计算得到磷的浓度。Add 10 mg Mg-Al/CSF meter per 10 mL of 100 mg/L potassium dihydrogen phosphate solution, adjust the pH of the solution to 3, and after adsorption for 2 h at a temperature of 25 °C, the phosphorus concentration is detected with a visible spectrophotometer at a wavelength of λ=700 nm , and calculate the phosphorus concentration.

所制备的吸附剂对磷的去除率达到58%。The phosphorus removal rate of the prepared adsorbent reached 58%.

实施例2Example 2

一种镁铝复合氧化物改性椰子壳生物质炭吸附材料的制备方法,包括如下步骤:A preparation method of magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material, comprising the following steps:

a)将粉碎的椰子壳浸泡在0.5M氢氧化钠溶液中,90℃条件下搅拌4h,去除杂质后,用去离子水洗涤,加入醋酸酸化的亚氯酸钠溶液(质量分数5%)中进行脱色处理,然后将脱色的生物质用去离子水清洗,烘干后得到椰子壳纤维;a) Soak the crushed coconut shells in 0.5M sodium hydroxide solution, stir at 90°C for 4 hours, remove impurities, wash with deionized water, add acetic acid acidified sodium chlorite solution (mass fraction 5%) Carry out decolorization treatment, then the decolorized biomass is washed with deionized water, and the coconut husk fiber is obtained after drying;

b)按照每100mL去离子水中溶解10g九水合硝酸铝计,将得到的椰子壳纤维浸泡8h后过滤,烘干得到的样品在氮气条件下450℃煅烧6h,得到氧化铝包覆的椰子壳纤维(Al2O3/CSF);b) Dissolving 10 g of aluminum nitrate nonahydrate per 100 mL of deionized water, soak the obtained coconut husk fibers for 8 hours and then filter them. The samples obtained by drying are calcined at 450° C. for 6 hours under nitrogen conditions to obtain alumina-coated coconut husk fibers. (Al 2 O 3 /CSF);

c)按照固液比0.6g:0.25g:0.2g:90mL,将六水合硝酸镁、Al2O3/CSF、六亚甲基四胺溶于去离子水中,充分搅拌后,将混合物转移到不锈钢反应釜中,90℃反应18h后,过滤、洗涤,烘干后的产物在氮气氛围下500℃煅烧6h,得到镁铝复合氧化物改性椰子壳生物质炭吸附材料(Mg-Al/CSF)。c) According to the solid-liquid ratio of 0.6g:0.25g:0.2g:90mL, dissolve magnesium nitrate hexahydrate, Al 2 O 3 /CSF and hexamethylenetetramine in deionized water, and after thorough stirring, transfer the mixture to a In a stainless steel reactor, after reacting at 90°C for 18h, filtered, washed, and the dried product was calcined at 500°C for 6h under nitrogen atmosphere to obtain magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material (Mg-Al/CSF ).

废水中磷的去除:Phosphorus removal from wastewater:

按每10mL 100mg/L的磷酸二氢钾溶液加入15mg Mg-Al/CSF计,调节溶液pH在7,温度30℃条件下吸附2h后,磷浓度用可见分光光度计在波长λ=700nm处检测,并计算得到磷的浓度。Add 15mg Mg-Al/CSF meter per 10mL of 100mg/L potassium dihydrogen phosphate solution, adjust the pH of the solution to 7, and after adsorption for 2h at a temperature of 30°C, the phosphorus concentration is detected with a visible spectrophotometer at a wavelength of λ=700nm , and calculate the phosphorus concentration.

所制备的吸附剂对磷的去除率达到66%。The phosphorus removal rate of the prepared adsorbent reached 66%.

实施例3Example 3

一种镁铝复合氧化物改性椰子壳生物质炭吸附材料的制备方法,包括如下步骤:A preparation method of magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material, comprising the following steps:

a)将粉碎的椰子壳浸泡在1M氢氧化钠溶液中,80℃条件下搅拌3h,去除杂质后,用去离子水洗涤,加入醋酸酸化的亚氯酸钠溶液(质量分数5%)中进行脱色处理,然后将脱色的生物质用去离子水清洗,烘干后得到椰子壳纤维;a) Soak the crushed coconut shells in 1M sodium hydroxide solution, stir at 80°C for 3 hours, remove impurities, wash with deionized water, add acetic acid acidified sodium chlorite solution (mass fraction 5%) to carry out Decolorization treatment, then the decolorized biomass is washed with deionized water, and the coconut husk fiber is obtained after drying;

b)按照每100mL去离子水中溶解5g九水合硝酸铝计,将得到的椰子壳纤维浸泡10h后过滤,烘干得到的样品在氮气条件下400℃煅烧4h,得到氧化铝包覆的椰子壳纤维(Al2O3/CSF);b) Dissolving 5 g of aluminum nitrate nonahydrate per 100 mL of deionized water, soak the obtained coconut husk fibers for 10 hours, filter them, and calcine the samples obtained by drying at 400° C. for 4 hours under nitrogen conditions to obtain alumina-coated coconut husk fibers. (Al 2 O 3 /CSF);

c)按照固液比0.9g:0.3g:0.5g:75mL,将六水合硝酸镁、Al2O3/CSF、六亚甲基四胺溶于去离子水中,充分搅拌后,将混合物转移到不锈钢反应釜中,120℃反应12h后,过滤、洗涤,烘干后的产物在氮气氛围下500℃煅烧4h,得到镁铝复合氧化物改性椰子壳生物质炭吸附材料(Mg-Al/CSF)。c) According to the solid-liquid ratio of 0.9g:0.3g:0.5g:75mL, dissolve magnesium nitrate hexahydrate, Al 2 O 3 /CSF, and hexamethylenetetramine in deionized water, and after thorough stirring, transfer the mixture to a In a stainless steel reactor, after reacting at 120 °C for 12 h, filtered, washed, and the dried product was calcined at 500 °C for 4 h under nitrogen atmosphere to obtain magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material (Mg-Al/CSF ).

废水中磷的去除:Phosphorus removal from wastewater:

按每10mL 100mg/L的磷酸二氢钾溶液加入25mg Mg-Al/CSF计,调节溶液pH在6,温度45℃条件下吸附2h后,磷浓度用可见分光光度计在波长λ=700nm处检测,并计算得到磷的浓度。Add 25mg Mg-Al/CSF meter per 10mL of 100mg/L potassium dihydrogen phosphate solution, adjust the pH of the solution to 6, after adsorption for 2h at a temperature of 45°C, the phosphorus concentration is detected with a visible spectrophotometer at wavelength λ=700nm , and calculate the phosphorus concentration.

所制备的吸附剂对磷的去除率达到94.5%。The phosphorus removal rate of the prepared adsorbent reached 94.5%.

实施例4Example 4

一种镁铝复合氧化物改性椰子壳生物质炭吸附材料的制备方法,包括如下步骤:A preparation method of magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material, comprising the following steps:

a)将粉碎的椰子壳浸泡在1.2M氢氧化钠溶液中,150℃条件下搅拌4h,去除杂质后,用去离子水洗涤,加入醋酸酸化的亚氯酸钠溶液(质量分数5%)中进行脱色处理,然后将脱色的生物质用去离子水清洗,烘干后得到椰子壳纤维;a) Soak the crushed coconut shells in 1.2M sodium hydroxide solution, stir at 150°C for 4 hours, remove impurities, wash with deionized water, and add to acetic acid acidified sodium chlorite solution (mass fraction 5%) Carry out decolorization treatment, then the decolorized biomass is washed with deionized water, and the coconut husk fiber is obtained after drying;

b)按照每100mL去离子水中溶解15g九水合硝酸铝计,将得到的椰子壳纤维浸泡16h后过滤,烘干得到的样品在氮气条件下350℃煅烧8h,得到氧化铝包覆的椰子壳纤维(Al2O3/CSF);b) Dissolving 15g of aluminum nitrate nonahydrate per 100mL of deionized water, soak the obtained coconut husk fibers for 16 hours, filter them, and calcine the obtained samples under nitrogen conditions at 350° C. for 8 hours to obtain alumina-coated coconut husk fibers (Al 2 O 3 /CSF);

c)按照固液比1.2g:0.6g:0.8g:100mL,将六水合硝酸镁、Al2O3/CSF、六亚甲基四胺溶于去离子水中,充分搅拌后,将混合物转移到不锈钢反应釜中,120℃反应24h后,过滤、洗涤,烘干后的产物在氮气氛围下600℃煅烧6h,得到镁铝复合氧化物改性椰子壳生物质炭吸附材料(Mg-Al/CSF)。c) According to the solid-liquid ratio of 1.2g:0.6g:0.8g:100mL, dissolve magnesium nitrate hexahydrate, Al 2 O 3 /CSF and hexamethylenetetramine in deionized water, and after thorough stirring, transfer the mixture to a In a stainless steel reactor, after reacting at 120°C for 24h, filtered, washed, and the dried product was calcined at 600°C for 6h under nitrogen atmosphere to obtain magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material (Mg-Al/CSF ).

废水中磷的去除:Phosphorus removal from wastewater:

按每10mL 100mg/L的磷酸二氢钾溶液加入30mg Mg-Al/CSF计,调节溶液pH在8,温度40℃条件下吸附2h后,磷浓度用可见分光光度计在波长λ=700nm处检测,并计算得到磷的浓度。Add 30 mg of Mg-Al/CSF meter per 10 mL of 100 mg/L potassium dihydrogen phosphate solution, adjust the pH of the solution to 8, and after adsorption for 2 h at a temperature of 40 °C, the phosphorus concentration is detected with a visible spectrophotometer at wavelength λ=700 nm , and calculate the phosphorus concentration.

所制备的吸附剂对磷的去除率达到78.5%。The phosphorus removal rate of the prepared adsorbent reached 78.5%.

实施例5Example 5

一种镁铝复合氧化物改性椰子壳生物质炭吸附材料的制备方法,包括如下步骤:A preparation method of magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material, comprising the following steps:

a)将粉碎的椰子壳浸泡在1.5M氢氧化钠溶液中,150℃条件下搅拌8h,去除杂质后,用去离子水洗涤,加入醋酸酸化的亚氯酸钠溶液(质量分数5%)中进行脱色处理,然后将脱色的生物质用去离子水清洗,烘干后得到椰子壳纤维;a) Soak the crushed coconut shells in 1.5M sodium hydroxide solution, stir at 150°C for 8 hours, remove impurities, wash with deionized water, and add to acetic acid acidified sodium chlorite solution (mass fraction 5%) Carry out decolorization treatment, then the decolorized biomass is washed with deionized water, and the coconut husk fiber is obtained after drying;

b)按照每100mL去离子水中溶解20g九水合硝酸铝计,将得到的椰子壳纤维浸泡20h后过滤,烘干得到的样品在氮气条件下800℃煅烧8h,得到氧化铝包覆的椰子壳纤维(Al2O3/CSF);b) Dissolving 20 g of aluminum nitrate nonahydrate per 100 mL of deionized water, soak the obtained coconut husk fibers for 20 hours, filter them, and calcine the obtained samples at 800°C for 8 hours under nitrogen conditions to obtain alumina-coated coconut husk fibers (Al 2 O 3 /CSF);

c)按照固液比1.8g:0.9g:1.0g:200mL,将六水合硝酸镁、Al2O3/CSF、六亚甲基四胺溶于去离子水中,充分搅拌后,将混合物转移到不锈钢反应釜中,180℃反应48h后,过滤、洗涤,烘干后的产物在氮气氛围下800℃煅烧8h,得到镁铝复合氧化物改性椰子壳生物质炭吸附材料(Mg-Al/CSF)。c) According to the solid-to-liquid ratio of 1.8g:0.9g:1.0g:200mL, dissolve magnesium nitrate hexahydrate, Al 2 O 3 /CSF, and hexamethylenetetramine in deionized water, and after thorough stirring, transfer the mixture to a In a stainless steel reactor, after reacting at 180 °C for 48 h, filtered, washed, and the dried product was calcined at 800 °C for 8 h under nitrogen atmosphere to obtain magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material (Mg-Al/CSF ).

废水中磷的去除:Phosphorus removal from wastewater:

按每10mL 100mg/L的磷酸二氢钾溶液加入40mg Mg-Al/CSF计,调节溶液pH在10,温度45℃条件下吸附2h后,磷浓度用可见分光光度计在波长λ=700nm处检测,并计算得到磷的浓度。Add 40 mg of Mg-Al/CSF meter per 10 mL of 100 mg/L potassium dihydrogen phosphate solution, adjust the pH of the solution to 10, and after adsorption for 2 h at a temperature of 45 °C, the phosphorus concentration is detected with a visible spectrophotometer at a wavelength of λ=700 nm , and calculate the phosphorus concentration.

所制备的吸附剂对磷的去除率达到83%。The phosphorus removal rate of the prepared adsorbent reached 83%.

以上所述仅为本发明的实施例,并非因此限制本发明的专利范围,凡是利用本发明说明书所作的等效结构或等效流程变换,或直接或间接运用在其他相关的技术领域,均同理包括在本发明的专利保护范围内。The above descriptions are only the embodiments of the present invention, and are not intended to limit the scope of the patent of the present invention. Any equivalent structure or equivalent process transformation made by the description of the present invention, or directly or indirectly applied in other related technical fields, are the same as The principles are included in the scope of patent protection of the present invention.

Claims (10)

1.一种镁铝复合氧化物改性椰子壳生物质炭吸附材料的制备方法,其特征在于,包括如下步骤:1. a preparation method of magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material, is characterized in that, comprises the steps: a) 将粉碎的椰子壳浸泡在氢氧化钠溶液中, 60~150℃条件下搅拌1~8 h,去除杂质后,用去离子水洗净,加入醋酸酸化的亚氯酸钠溶液中进行脱色处理,然后将脱色的生物质用去离子水清洗,烘干后得到椰子壳纤维;a) Soak the crushed coconut shells in sodium hydroxide solution, stir at 60~150℃ for 1~8 h, remove impurities, wash with deionized water, add acetic acid acidified sodium chlorite solution to decolorize Treatment, then the decolorized biomass is washed with deionized water, and the coconut husk fiber is obtained after drying; b) 按照每100 mL去离子水中溶解1~20 g九水合硝酸铝计,将得到的椰子壳纤维浸泡5~20 h后过滤,烘干得到的样品在氮气氛围中200~800℃煅烧2~8 h,得到氧化铝包覆的椰子壳纤维Al2O3/CSF;b) Calculated by dissolving 1-20 g aluminum nitrate nonahydrate per 100 mL of deionized water, soak the obtained coconut husk fiber for 5-20 h, filter it, and calcine the obtained sample at 200-800 ℃ for 2-20 hours in a nitrogen atmosphere. 8 h to obtain alumina-coated coconut husk fiber Al 2 O 3 /CSF; c) 按照固液比0.3~1.8 g : 0.1~0.9 g : 0.05~1.0 g : 50~200 mL,将六水合硝酸镁、Al2O3/CSF、六亚甲基四胺溶于去离子水中,充分搅拌后,将混合物转移到不锈钢反应釜中,60~180℃反应6~48 h后,过滤、洗涤,烘干后的产物在氮气氛围中200~800℃煅烧2~8 h,即得。c) According to the solid-liquid ratio of 0.3~1.8 g : 0.1~0.9 g : 0.05~1.0 g : 50~200 mL, dissolve magnesium nitrate hexahydrate, Al 2 O 3 /CSF and hexamethylenetetramine in deionized water , after fully stirring, the mixture was transferred to a stainless steel reactor, reacted at 60-180 °C for 6-48 h, filtered, washed, and the dried product was calcined at 200-800 °C for 2-8 h in a nitrogen atmosphere to obtain . 2.根据权利要求1所述镁铝复合氧化物改性椰子壳生物质炭吸附材料的制备方法,其特征在于:步骤a)中所述氢氧化钠溶液浓度为0.2~1.5 M ,所述醋酸酸化的亚氯酸钠溶液,是将亚氯酸钠按照5%质量分数溶于水再以醋酸调节pH为4。2. The preparation method of the magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material according to claim 1, wherein the concentration of the sodium hydroxide solution in step a) is 0.2-1.5 M, and the acetic acid The acidified sodium chlorite solution is made by dissolving sodium chlorite in water according to 5% mass fraction and adjusting the pH to 4 with acetic acid. 3.根据权利要求1所述镁铝复合氧化物改性椰子壳生物质炭吸附材料的制备方法,其特征在于:步骤a)中所述将粉碎的椰子壳浸泡在1 M氢氧化钠溶液中, 80℃条件下搅拌3h。3. The preparation method of magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material according to claim 1, characterized in that: described in step a), the pulverized coconut shell is soaked in 1 M sodium hydroxide solution , and stirred at 80°C for 3h. 4.根据权利要求1所述镁铝复合氧化物改性椰子壳生物质炭吸附材料的制备方法,其特征在于:步骤b)中所述按照每100 mL去离子水中溶解5 g九水合硝酸铝计,将得到的椰子壳纤维浸泡10 h后过滤。4. the preparation method of magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material according to claim 1, is characterized in that: according to every 100 mL of deionized water in step b), dissolve 5 g of aluminum nitrate nonahydrate according to The obtained coconut husk fibers were soaked for 10 h and filtered. 5.根据权利要求1所述镁铝复合氧化物改性椰子壳生物质炭吸附材料的制备方法,其特征在于:步骤b)中所述烘干得到的样品在氮气氛围中400℃煅烧4 h。5. The preparation method of the magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material according to claim 1, wherein the sample obtained by drying in step b) is calcined at 400°C for 4 h in a nitrogen atmosphere . 6.根据权利要求1所述镁铝复合氧化物改性椰子壳生物质炭吸附材料的制备方法,其特征在于:步骤c)中所述按照固液比0.9 g : 0.3 g : 0.5 g : 75 mL,将六水合硝酸镁、Al2O3/CSF、六亚甲基四胺溶于去离子水中。6. the preparation method of magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material according to claim 1, is characterized in that: described in step c) according to solid-liquid ratio 0.9 g: 0.3 g: 0.5 g: 75 mL, magnesium nitrate hexahydrate, Al 2 O 3 /CSF, hexamethylenetetramine were dissolved in deionized water. 7.根据权利要求1所述镁铝复合氧化物改性椰子壳生物质炭吸附材料的制备方法,其特征在于:步骤c)中所述将混合物转移到不锈钢反应釜中,120℃反应12 h。7. The preparation method of magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material according to claim 1, wherein the mixture is transferred to a stainless steel reactor as described in step c), and the reaction is carried out at 120°C for 12 h . 8.根据权利要求1所述镁铝复合氧化物改性椰子壳生物质炭吸附材料的制备方法,其特征在于:步骤c)中所述烘干后的产物在氮气氛围中500℃煅烧4 h。8. The preparation method of magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material according to claim 1, characterized in that: the product after drying described in step c) is calcined at 500 ° C for 4 h in a nitrogen atmosphere . 9.根据权利要求1-8任一所述方法制备得到的镁铝复合氧化物改性椰子壳生物质炭吸附材料。9. The magnesium-aluminum composite oxide modified coconut shell biomass charcoal adsorption material prepared according to any one of claims 1-8. 10.一种如权利要求9所述镁铝复合氧化物改性椰子壳生物质炭吸附材料的应用,其特征在于:将其应用于废水除磷。10. An application of the magnesium-aluminum composite oxide modified coconut shell biomass carbon adsorption material as claimed in claim 9, characterized in that: it is applied to the phosphorus removal of waste water.
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