CN106378087B - The preparation method of nano composite adsorption material, adsorbent and processing method for handling trihydroxy triphenylmenthane substance in waste water - Google Patents
The preparation method of nano composite adsorption material, adsorbent and processing method for handling trihydroxy triphenylmenthane substance in waste water Download PDFInfo
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
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- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
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- B01J20/043—Carbonates or bicarbonates, e.g. limestone, dolomite, aragonite
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- C—CHEMISTRY; METALLURGY
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- C02F1/00—Treatment of water, waste water, or sewage
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Abstract
Description
技术领域technical field
本发明属于吸附材料技术领域，具体涉及纳米复合吸附材料的制备方法、用于处理废水中三羟基三苯甲烷类物质的吸附剂及处理方法。The invention belongs to the technical field of adsorption materials, and in particular relates to a preparation method of nanocomposite adsorption materials, an adsorbent for treating trihydroxytriphenylmethane substances in waste water and a treatment method.
背景技术Background technique
社会经济的迅速发展导致水环境污染日益突出。目前，用于废水处理的主要技术有活性污泥法、膜分离法、电化学法等。其中以吸附材料为基础的吸附法因处理污染物效率高、操作费用少、处理速度快、适应性强等特点至今仍被广泛使用。The rapid development of social economy has led to increasingly prominent water environment pollution. At present, the main technologies used for wastewater treatment include activated sludge method, membrane separation method, electrochemical method and so on. Among them, the adsorption method based on adsorption materials is still widely used because of its high efficiency in treating pollutants, low operating costs, fast processing speed, and strong adaptability.
传统的吸附材料主要有活性炭、活性氧化铝、硅藻土、沸石、硅藻土、壳聚糖、吸附树脂等。但这些吸附材料普遍存在吸附无选择性、再生困难、吸附容量低等缺陷。纳米材料比表面积大的特点使其成为新型吸附材料的首选，且纳米材料随着粒子直径的减小，比表面积迅速增加，吸附效果越好，如何制备粒径小的纳米材料是其成为吸附材料的关键，纳米材料的选择吸附性也是决定其吸附性能的重要指标。但目前尚没有性能优异的纳米吸附材料存在，因此，研究人员仍在针对以上材料缺陷寻找高效、专一的新型吸附材料。Traditional adsorption materials mainly include activated carbon, activated alumina, diatomite, zeolite, diatomite, chitosan, and adsorption resins. However, these adsorbents generally have defects such as non-selective adsorption, difficult regeneration, and low adsorption capacity. The large specific surface area of nanomaterials makes them the first choice for new adsorption materials, and as the particle diameter decreases, the specific surface area of nanomaterials increases rapidly, and the better the adsorption effect, how to prepare nanomaterials with small particle sizes is the key to becoming an adsorption material. The key to the selective adsorption of nanomaterials is also an important indicator to determine its adsorption performance. However, there is no nano-adsorption material with excellent performance at present. Therefore, researchers are still looking for efficient and specific new adsorption materials for the above material defects.
发明内容Contents of the invention
针对现有技术存在的上述不足，本发明要解决的技术问题是：针对现有技术中吸附材料吸附无选择性、吸附容量低的问题，而提供一种吸附容量高、选择性好的纳米复合吸附材料的制备方法、用于处理废水中三羟基三苯甲烷类物质的吸附剂及处理方法。Aiming at the above-mentioned deficiencies in the prior art, the technical problem to be solved by the present invention is to provide a nanocomposite nanocomposite with high adsorption capacity and good selectivity for the problems of non-selective adsorption and low adsorption capacity of the adsorption material in the prior art. A preparation method of an adsorption material, an adsorbent for treating trihydroxytriphenylmethane substances in waste water and a treatment method.
为了解决上述技术问题，本发明采用如下技术方案：一种纳米复合吸附材料的制备方法，包括如下步骤：In order to solve the above-mentioned technical problems, the present invention adopts the following technical scheme: a preparation method of a nanocomposite adsorption material, comprising the steps of:
1）以SrCO3、Bi(NO3)3·5H2O和C3H6N6为混合原料，将所述混合原料溶于水中配成混合溶液；其中，所述SrCO3、Bi(NO3)3·5H2O和C3H6N6的质量比为1~3：1~5：1~10；1) Using SrCO 3 , Bi(NO 3 ) 3 ·5H 2 O and C 3 H 6 N 6 as mixed raw materials, the mixed raw materials were dissolved in water to form a mixed solution; wherein, the SrCO 3 , Bi(NO 3 ) The mass ratio of 3 5H 2 O to C 3 H 6 N 6 is 1~3:1~5:1~10;
2）将步骤1）配制的混合溶液置于60~80℃下烘干1~2 h，得到烘干混合材料；2) Dry the mixed solution prepared in step 1) at 60-80°C for 1-2 hours to obtain the dried mixed material;
3）将步骤2）得到的烘干混合材料于400~700℃下煅烧4~6 h，得到煅烧材料；3) Calcining the dried mixed material obtained in step 2) at 400-700°C for 4-6 hours to obtain a calcined material;
4）对步骤3）得到的煅烧材料进行粉碎处理，得到所述纳米复合吸附材料。4) Pulverizing the calcined material obtained in step 3) to obtain the nanocomposite adsorption material.
现有技术中类石墨型氮化碳（Graphitic carbon nitride，g-C3N4）聚合物具有与石墨类似的层状结构，层上是由C3N3环或C6N7环构成，环之间通过N原子相连形成一层无限扩展的平面，层与层之间则是由弱的范德华力结合起来，大多数无机化合物和无机金属离子能够结合或者插入到g-C3N4基质中，改变其固有性质，提高其在催化领域的使用范畴，常被用作光催化剂领域。SrCO3被广泛用于彩电阴极射线管、电磁铁、锶铁氧体等领域，铋系化合物具有优越的光催化性能而被前人常用来研究作为光催化剂。目前为止本领域技术人员都是重点关注上述是三种材料的光催化性能）并没有过采用类石墨型氮化碳、SrCO3和铋系化合物制备纳米吸附材料的相关研究，现有技术中也没有相关研究证明类石墨型氮化碳、SrCO3和铋系化合物可以用作吸附剂制备原料用来制备具有优异吸附功能的纳米吸附材料。本发明突破现有技术中类石墨型氮化碳、SrCO3和铋系化合物仅作为光催化剂原料的常规认识，在研究类石墨型氮化碳、SrCO3和铋系化合物三种材料复合制作光催化材料时偶然发现制得的材料不具有很好的光催化性能，却具有突出的吸附功效，研究发现基于g-C3N4的层状结构以及SrCO3、铋系化合物具备的特殊性能，通过煅烧的方法改变了材料的晶型结构、表面基团等，以使该复合体系具有优良的吸附容量，尤其对废水中的有机染料具有良好的选择吸附效果，取得了意想不到的纳米吸附效果。In the prior art, graphite-like carbon nitride (Graphitic carbon nitride, gC 3 N 4 ) polymer has a layered structure similar to graphite, and the layer is composed of C3N3 rings or C6N7 rings, and the rings are connected by N atoms to form A layer of infinitely extended plane, and the layers are combined by weak van der Waals force. Most inorganic compounds and inorganic metal ions can be combined or inserted into the gC 3 N 4 matrix to change its inherent properties and improve its The scope of use in the field of catalysis is often used in the field of photocatalysis. SrCO 3 is widely used in color TV cathode ray tubes, electromagnets, strontium ferrite and other fields. Bismuth compounds have excellent photocatalytic properties and are often used as photocatalysts by predecessors. So far, those skilled in the art have all focused on the photocatalytic properties of the above-mentioned three materials) and have not used graphitic carbon nitride, SrCO 3 and bismuth-based compounds to prepare nano-adsorption materials. In the prior art, there are also There is no relevant research to prove that graphite-like carbon nitride, SrCO 3 and bismuth-based compounds can be used as raw materials for the preparation of adsorbents to prepare nano-adsorption materials with excellent adsorption functions. The present invention breaks through the conventional understanding that graphite-like carbon nitride, SrCO 3 and bismuth-based compounds are only used as photocatalyst raw materials in the prior art. When using catalytic materials, it was accidentally found that the prepared materials did not have good photocatalytic performance, but had outstanding adsorption effects. The study found that based on the layered structure of gC 3 N 4 and the special properties of SrCO 3 and bismuth compounds, through calcination The method changes the crystal structure and surface groups of the material, so that the composite system has excellent adsorption capacity, especially for organic dyes in wastewater, and has achieved unexpected nano-adsorption effects.
进一步，步骤1）中所述混合原料的总质量与所述水的质量体积比≥1:10。这样的用量，可以既满足使混合原料更均匀地分散混合在水中的要求，又避免了用水量过多导致的后续干燥时间过长的问题。Further, the mass volume ratio of the total mass of the mixed raw materials to the water in step 1) is ≥1:10. Such an amount can not only meet the requirements of making the mixed raw materials more uniformly dispersed and mixed in water, but also avoid the problem of too long subsequent drying time caused by excessive water consumption.
进一步，步骤1）中将所述混合原料置于水中超声分散处理10~20 min，配成混合溶液。采用超声分散处理的方法，可以有效提高分散效率，使溶质更加充分彻底地溶解在混合溶液中，混合性能更好。Further, in step 1), the mixed raw materials are placed in water for ultrasonic dispersion treatment for 10-20 min to form a mixed solution. The method of ultrasonic dispersion treatment can effectively improve the dispersion efficiency, make the solute more fully and thoroughly dissolve in the mixed solution, and the mixing performance is better.
进一步，步骤1）中所述SrCO3、Bi(NO3)3·5H2O和C3H6N6的质量比为1:1:3。采用这样的质量比，可以使得到的吸附材料对三羟基三苯甲烷类物质的吸附效果更好，对结晶紫的吸附效果可达93.85%，取得了优异的吸附效果。Further, the mass ratio of SrCO 3 , Bi(NO 3 ) 3 ·5H 2 O and C 3 H 6 N 6 in step 1) is 1:1:3. With such a mass ratio, the obtained adsorption material can have a better adsorption effect on trihydroxytriphenylmethane substances, and the adsorption effect on crystal violet can reach 93.85%, and an excellent adsorption effect has been achieved.
作为优化，步骤3）中将烘干混合材料于550℃下煅烧4 h。采用这样的煅烧时间和煅烧温度，可以使复合材料煅烧后的晶型结构更加能够满足高吸附效果的要求。As an optimization, in step 3), the dried mixed material was calcined at 550 °C for 4 h. By adopting such calcination time and calcination temperature, the crystalline structure of the composite material after calcination can better meet the requirement of high adsorption effect.
一种用于处理废水中三羟基三苯甲烷类物质的吸附剂，其组分包括上述方法制得的纳米复合吸附材料。这样的废水处理用吸附剂相较于现有技术中的活性炭、硅藻土等吸附剂选择吸附性更强，尤其对废水中的三羟基三苯甲烷类物质具有高选择吸附性，对印染废水中的各种结晶紫等三羟基三苯甲烷类物质吸附容量高，处理效果好，相较于现有印染废水中三羟基三苯甲烷类物质处理用吸附剂取得了意想不到的吸附处理效果。An adsorbent for treating trihydroxytriphenylmethane substances in waste water, the components of which include the nanocomposite adsorbent material prepared by the above method. Compared with adsorbents such as activated carbon and diatomaceous earth in the prior art, such adsorbents for wastewater treatment have stronger selective adsorption properties, especially for trihydroxytriphenylmethane substances in wastewater, and have higher selective adsorption properties for printing and dyeing wastewater. Various crystal violet and other trihydroxytriphenylmethane substances in the method have high adsorption capacity and good treatment effect. Compared with the existing adsorbents for the treatment of trihydroxytriphenylmethane substances in printing and dyeing wastewater, unexpected adsorption treatment effects have been achieved.
一种废水中三羟基三苯甲烷类物质的处理方法，将所述用于处理废水中三羟基三苯甲烷类物质的吸附剂投加入废水中处理15~120 min；其中，所述吸附剂与废水的质量体积比为0.2~1.0 g：1000 mL。按照这样的处理方法对废水中的三羟基三苯甲烷类物质进行吸附处理，既保证了吸附处理效果好，又缩短了现有废水中三羟基三苯甲烷类物质的处理时间，具有良好的市场前景。A method for treating trihydroxytriphenylmethane substances in wastewater, wherein the adsorbent for treating trihydroxytriphenylmethane substances in wastewater is added to the wastewater for treatment for 15 to 120 min; wherein, the adsorbent and The mass volume ratio of wastewater is 0.2~1.0 g:1000 mL. According to such a treatment method, the trihydroxytriphenylmethane substances in the wastewater are adsorbed, which not only ensures a good adsorption treatment effect, but also shortens the treatment time of the trihydroxytriphenylmethane substances in the existing wastewater, and has a good market prospect.
作为优化，所述吸附剂与废水的质量体积比为1.0 g：1000 mL，处理时间为90min。这样的处理条件下，吸附效果最好。As an optimization, the mass volume ratio of the adsorbent to the waste water is 1.0 g:1000 mL, and the treatment time is 90 min. Under such treatment conditions, the adsorption effect is the best.
作为优化，所述有机染料为结晶紫。本发明方法对结晶紫的去除效果最好，对结晶紫的吸附效率高达93.85%。As an optimization, the organic dye is crystal violet. The method of the invention has the best removal effect on crystal violet, and the adsorption efficiency on crystal violet is as high as 93.85%.
相比现有技术，本发明具有如下有益效果：本发明方法突破现有技术中类石墨型氮化碳、SrCO3和铋系化合物仅作为光催化剂原料的常规认识，基于g-C3N4的层状结构以及SrCO3、铋系化合物的协同配伍作用，煅烧制得了具有高选择性、高吸附容量的纳米吸附材料，该纳米吸附材料对废水中的三羟基三苯甲烷类物质选择吸附性强、吸附效果好，尤其对结晶紫的吸附率高达93.85%，取得了意想不到的吸附处理效果。且本发明方法制备过程简单，用于废水处理时操作便捷、处理时间短，具有良好的工业化生产和市场应用前景。Compared with the prior art, the present invention has the following beneficial effects: the method of the present invention breaks through the conventional understanding that graphite-like carbon nitride, SrCO 3 and bismuth compounds are only used as photocatalyst raw materials in the prior art, and the layer based on gC 3 N 4 Like structure and the synergistic compatibility of SrCO 3 and bismuth compounds, the nano-adsorption material with high selectivity and high adsorption capacity was obtained by calcination. The nano-adsorption material has strong selective adsorption for trihydroxytriphenylmethane substances in wastewater, The adsorption effect is good, especially the adsorption rate of crystal violet is as high as 93.85%, and an unexpected adsorption treatment effect has been achieved. Moreover, the method of the invention has simple preparation process, convenient operation and short treatment time when used for wastewater treatment, and has good industrialized production and market application prospects.
具体实施方式Detailed ways
下面结合具体实施例对本发明作进一步详细说明。本实施案例在以本发明技术为前提下进行实施，现给出详细的实施方式和具体的操作过程来说明本发明具有创造性，但本发明的保护范围不限于以下的实施例。The present invention will be described in further detail below in conjunction with specific embodiments. This implementation case is carried out on the premise of the technology of the present invention, and the detailed implementation and specific operation process are given to illustrate the inventiveness of the present invention, but the protection scope of the present invention is not limited to the following examples.
实施例1：Example 1:
一种纳米复合吸附材料的制备方法，包括如下步骤：A preparation method of nanocomposite adsorption material, comprising the steps of:
1）分别取4.5 g SrCO3、4.5g Bi(NO3)3·5H2O、9.0g C3H6N6作为混合原料，将混合原料溶于15 mL去离子水中，然后超声分散15 min使其混合均匀，得到混合溶液。1) Take 4.5 g SrCO 3 , 4.5 g Bi(NO 3 ) 3 5H 2 O, and 9.0 g C 3 H 6 N 6 as mixed raw materials, dissolve the mixed raw materials in 15 mL deionized water, and then ultrasonically disperse them for 15 min It was mixed uniformly to obtain a mixed solution.
2）将步骤1）得到的混合溶液置于60℃烘箱中，烘干1.5 h，以去除混合溶液中的多余水分，得到烘干混合材料。2) Put the mixed solution obtained in step 1) in an oven at 60°C for 1.5 h to remove excess water in the mixed solution and obtain a dried mixed material.
3）将步骤2）烘干混合材料置于马弗炉中煅烧，温度设定为550℃，煅烧时间为4h，得到煅烧材料。3) The dried mixed material in step 2) was calcined in a muffle furnace, the temperature was set at 550° C., and the calcined time was 4 hours to obtain the calcined material.
4）待步骤3）得到的煅烧材料冷却至室温后，用研钵研细后，即得制备的纳米复合吸附材料。4) After the calcined material obtained in step 3) is cooled to room temperature, it is finely ground with a mortar to obtain the prepared nanocomposite adsorption material.
本实施例还提供了一种用于处理废水中三羟基三苯甲烷类物质的吸附剂，其组分为本实施例上述方法制得的纳米复合吸附材料。This embodiment also provides an adsorbent for treating trihydroxytriphenylmethane substances in wastewater, the component of which is the nanocomposite adsorption material prepared by the above method in this embodiment.
将该用于处理废水中三羟基三苯甲烷类物质的吸附剂投加入10 mg/L的结晶紫溶液（模拟含有有机染料的废水）中，所述吸附剂与结晶紫溶液的质量体积比为1.0g：1000mL，在25℃下对结晶紫溶液进行吸附处理135 min，结果显示采用这样的处理方法，对结晶紫的吸附效率可高达93.85%，取得了突出的选择吸附性和高吸附容量效果。The adsorbent used to treat trihydroxytriphenylmethane substances in wastewater was added to 10 mg/L crystal violet solution (simulating wastewater containing organic dyes), and the mass volume ratio of the adsorbent to crystal violet solution was 1.0g: 1000mL, the crystal violet solution was adsorbed at 25°C for 135 minutes. The results showed that the adsorption efficiency of crystal violet could be as high as 93.85% with this treatment method, and outstanding selective adsorption and high adsorption capacity effects were achieved. .
实施例2：Example 2:
一种纳米复合吸附材料的制备方法，包括如下步骤：A preparation method of nanocomposite adsorption material, comprising the steps of:
1）分别取2.0 g SrCO3、2.0 g Bi(NO3)3·5H2O、14.0 g C3H6N6作为混合原料，将混合原料溶于20 mL去离子水中，然后超声分散20 min使其混合均匀，得到混合溶液。1) Take 2.0 g SrCO 3 , 2.0 g Bi(NO 3 ) 3 5H 2 O, and 14.0 g C 3 H 6 N 6 as mixed raw materials, dissolve the mixed raw materials in 20 mL deionized water, and then ultrasonically disperse them for 20 min It was mixed uniformly to obtain a mixed solution.
2）将步骤1）得到的混合溶液置于80℃烘箱中，烘干2 h，以去除混合溶液中的多余水分，得到烘干混合材料。2) Put the mixed solution obtained in step 1) in an oven at 80°C and dry for 2 hours to remove excess water in the mixed solution and obtain a dried mixed material.
3）将步骤2）烘干混合材料置于马弗炉中煅烧，温度设定为550℃，煅烧时间为4h，得到煅烧材料。3) The dried mixed material in step 2) was calcined in a muffle furnace, the temperature was set at 550° C., and the calcined time was 4 hours to obtain the calcined material.
4）待步骤3）得到的煅烧材料冷却至室温后，用研钵研细，即得制备的纳米复合吸附材料。4) After the calcined material obtained in step 3) is cooled to room temperature, grind it finely with a mortar to obtain the prepared nanocomposite adsorption material.
本实施例还提供了一种用于处理废水中三羟基三苯甲烷类物质的吸附剂，其组分为本实施例上述方法制得的纳米复合吸附材料。This embodiment also provides an adsorbent for treating trihydroxytriphenylmethane substances in wastewater, the component of which is the nanocomposite adsorption material prepared by the above method in this embodiment.
将该用于处理废水中三羟基三苯甲烷类物质的吸附剂投加入10 mg/L的结晶紫溶液（模拟含有有机染料的废水）中，所述吸附剂与结晶紫溶液的质量体积比为1.0g：1000mL，在25℃下对结晶紫溶液进行吸附处理135 min，结果显示采用这样的处理方法，对结晶紫的吸附效率可高达85.24%，取得了突出的选择吸附性和高吸附容量效果。The adsorbent used to treat trihydroxytriphenylmethane in wastewater was added to 10 mg/L crystal violet solution (simulating wastewater containing organic dyes), and the mass volume ratio of the adsorbent to crystal violet solution was 1.0g: 1000mL, the crystal violet solution was adsorbed at 25°C for 135 minutes. The results showed that the adsorption efficiency of crystal violet could be as high as 85.24% with this treatment method, and outstanding selective adsorption and high adsorption capacity effects were achieved. .
最后说明的是，以上实施例仅用以说明本发明的技术方案而非限制，尽管参照较佳实施例对本发明进行了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的宗旨和范围，其均应涵盖在本发明的权利要求范围当中。Finally, it is noted that the above embodiments are only used to illustrate the technical solutions of the present invention without limitation. Although the present invention has been described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that the technical solutions of the present invention can be carried out Modifications or equivalent replacements without departing from the spirit and scope of the technical solution of the present invention shall be covered by the claims of the present invention.
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