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CN117299095A - A binary compound lignin-based airgel adsorption material and its preparation method and application - Google Patents

A binary compound lignin-based airgel adsorption material and its preparation method and application Download PDF

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CN117299095A
CN117299095A CN202311494873.8A CN202311494873A CN117299095A CN 117299095 A CN117299095 A CN 117299095A CN 202311494873 A CN202311494873 A CN 202311494873A CN 117299095 A CN117299095 A CN 117299095A
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房大维
胡现珂
康莹
金子恒
魏杰
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Liaoning University
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Abstract

本发明属于水处理技术领域,具体涉及一种二元复配木质素基气凝胶吸附材料及其制备方法和应用。所述二元复配木质素基气凝胶吸附材料由木质素磺酸盐和羧基木聚糖进行复配,并与丙烯酰胺、交联剂、引发剂及四甲基乙二胺聚合、冷冻干燥制得。本发明采用绿色无毒、来源广泛的工业废弃物木质素磺酸盐为原料,利用其芳香特性及磺酸基阴离子复配羧基木聚糖进行协同吸附,通过简单的溶液共混与冷冻干燥获得了气凝胶吸附材料,具有成本低、环境友好、合成工艺简单、操作安全的优势,可应用于印染废水中亚甲基蓝的高效去除。The invention belongs to the technical field of water treatment, and specifically relates to a binary compound lignin-based airgel adsorption material and its preparation method and application. The binary compound lignin-based airgel adsorbent material is compounded of lignin sulfonate and carboxyxylan, and polymerized and frozen with acrylamide, cross-linking agent, initiator and tetramethylethylenediamine. Produced by drying. The invention uses green, non-toxic and widely sourced industrial waste lignosulfonate as raw material, utilizes its aromatic properties and sulfonic acid group anions to compound carboxyxylan for collaborative adsorption, and obtains it through simple solution blending and freeze-drying. The airgel adsorption material has the advantages of low cost, environmental friendliness, simple synthesis process, and safe operation, and can be applied to the efficient removal of methylene blue from printing and dyeing wastewater.

Description

一种二元复配木质素基气凝胶吸附材料及其制备方法和应用A binary compound lignin-based airgel adsorption material and its preparation method and application

技术领域Technical field

本发明属于水处理技术领域,具体涉及一种二元复配木质素基气凝胶吸附材料及其制备方法和应用。The invention belongs to the technical field of water treatment, and specifically relates to a binary compound lignin-based airgel adsorption material and its preparation method and application.

背景技术Background technique

亚甲基蓝是一种对人体有害的有机污染物,开发高效的水处理技术以去除印染废水中的亚甲基蓝,对于解决水体污染、维护人类生活环境健康具有重要的意义。与絮凝法、沉淀法、氧化法等水处理技术相比,吸附法由于操作简单、无污染,有望大规模应用于印染废水的处理。然而,目前常用的吸附材料吸附速率低、不易再生。相比之下,气凝胶具有低密度、高比表面积、高孔隙率和孔体积等优点,在吸附领域中具有广阔的应用前景。然而,传统无机与有机气凝胶的制备常涉及酸、碱及有机试剂等有毒有害试剂的应用,对生态环境及人体健康形成一定的危害作用,且成本较高,限制了其工业应用。因此,寻找一种绿色无毒、环境友好且成本低廉的气凝胶材料是废水处理领域的研究重点。Methylene blue is an organic pollutant that is harmful to the human body. The development of efficient water treatment technology to remove methylene blue from printing and dyeing wastewater is of great significance for solving water pollution and maintaining the health of the human living environment. Compared with water treatment technologies such as flocculation, precipitation, and oxidation, the adsorption method is expected to be widely used in the treatment of printing and dyeing wastewater due to its simple operation and no pollution. However, currently commonly used adsorbent materials have low adsorption rates and are difficult to regenerate. In contrast, aerogels have the advantages of low density, high specific surface area, high porosity and pore volume, and have broad application prospects in the field of adsorption. However, the preparation of traditional inorganic and organic aerogels often involves the application of toxic and harmful reagents such as acids, alkalis and organic reagents, which has a certain harmful effect on the ecological environment and human health, and the cost is high, limiting its industrial application. Therefore, finding a green, non-toxic, environmentally friendly and low-cost aerogel material is a research focus in the field of wastewater treatment.

木质素是自然界中丰富的可再生有机碳资源,主要存在于造纸等工业废弃物中,具备绿色无毒、生物相容性好、可降解且价格低廉的优势。此外,木质素富含芳香结构,其结构中含有丰富的功能基团如甲氧基、羰基、酚羟基等,反应活性高,是理想的气凝胶合成材料。目前,已有的用于水体中亚甲基蓝吸附的木质素基气凝胶材料多采用氧化石墨烯与木质素复合制备。如Li等(International Journal of Biological Macromolecules,2020,143,325-333)采用氧化石墨烯与碱木质素复合制备了气凝胶吸附材料,Li等(International Journal of Biological Macromolecules,2019,136,927-935)采用氧化石墨烯与木质素磺酸盐及壳聚糖复合制备了气凝胶吸附材料。然而,氧化石墨烯制备过程复杂,且涉及到强氧化剂高锰酸钾及过氧化氢的使用,造成一定的操作安全隐患。因此,对于亚甲基蓝废水处理,需要开发合成工艺简单且操作安全的高效木质素基气凝胶吸附材料。Lignin is an abundant renewable organic carbon resource in nature, mainly found in industrial wastes such as papermaking. It has the advantages of being green, non-toxic, biocompatible, degradable and low-priced. In addition, lignin is rich in aromatic structures, and its structure contains rich functional groups such as methoxy groups, carbonyl groups, phenolic hydroxyl groups, etc., and has high reactivity, making it an ideal aerogel synthetic material. At present, existing lignin-based aerogel materials used for the adsorption of methylene blue in water are mostly prepared by composites of graphene oxide and lignin. For example, Li et al. (International Journal of Biological Macromolecules, 2020, 143, 325-333) used graphene oxide and alkali lignin to composite to prepare airgel adsorption materials. Li et al. (International Journal of Biological Macromolecules, 2019, 136, 927- 935) used graphene oxide, lignosulfonate and chitosan to prepare airgel adsorption materials. However, the preparation process of graphene oxide is complicated and involves the use of strong oxidants potassium permanganate and hydrogen peroxide, causing certain operational safety hazards. Therefore, for methylene blue wastewater treatment, it is necessary to develop efficient lignin-based airgel adsorption materials with simple synthesis process and safe operation.

发明内容Contents of the invention

针对上述需求,本发明开发了一种二元复配木质素基气凝胶吸附材料。针对目标污染物结构特性,采用木质素磺酸盐为原料,复配羧基化木聚糖,协同吸附水体中亚甲基蓝。本发明采用环境友好的生物质原料,通过简单的溶液共混与冷冻干燥即可获得气凝胶材料,具备合成工艺简单、操作安全、绿色无毒、成本低廉的特点,可以更好地满足人们对于气凝胶吸附材料的需求。In response to the above needs, the present invention developed a binary compound lignin-based airgel adsorption material. In view of the structural characteristics of the target pollutants, lignosulfonate is used as raw material and compounded with carboxylated xylan to collaboratively adsorb methylene blue in water. The invention uses environmentally friendly biomass raw materials, and can obtain airgel materials through simple solution blending and freeze-drying. It has the characteristics of simple synthesis process, safe operation, green and non-toxic, and low cost, and can better meet people's needs. Demand for airgel adsorbent materials.

本发明采用的技术方案是:The technical solution adopted by the present invention is:

一种二元复配木质素基气凝胶吸附材料,由1.0-5.0wt%的木质素磺酸盐、0-10.0wt%的羧基木聚糖、5.0-20.0wt%的丙烯酰胺、1.0-5.0wt%的交联剂、0.5-2.5wt%的引发剂及0.5-2.5wt%的四甲基乙二胺反应制成。A binary compound lignin-based airgel adsorption material, consisting of 1.0-5.0wt% lignosulfonate, 0-10.0wt% carboxyxylan, 5.0-20.0wt% acrylamide, 1.0- It is made by reacting 5.0wt% cross-linking agent, 0.5-2.5wt% initiator and 0.5-2.5wt% tetramethylethylenediamine.

进一步的,上述的一种二元复配木质素基气凝胶吸附材料,所述木质素磺酸盐为木质素磺酸钠和木质素磺酸钙中的一种或两种的组合。Further, in the above-mentioned binary compound lignin-based airgel adsorption material, the lignosulfonate is one or a combination of two of sodium lignosulfonate and calcium lignosulfonate.

进一步的,上述的一种二元复配木质素基气凝胶吸附材料,所述羧基木聚糖为羧甲基木聚糖或羧乙基木聚糖。Further, in the above-mentioned binary compound lignin-based airgel adsorption material, the carboxyxylan is carboxymethylxylan or carboxyethylxylan.

进一步的,上述的一种二元复配木质素基气凝胶吸附材料,所述交联剂为N,N’-亚甲基双丙烯酰胺或氢氧化铝。Further, in the above-mentioned binary compound lignin-based airgel adsorption material, the cross-linking agent is N, N’-methylene bisacrylamide or aluminum hydroxide.

进一步的,上述的一种二元复配木质素基气凝胶吸附材料,所述引发剂为过氧化氢、过硫酸铵、过硫酸钾、过氧化苯甲酰、过氧化苯甲酰叔丁酯和过氧化甲乙酮中的一种。Further, the above-mentioned binary compound lignin-based airgel adsorption material, the initiator is hydrogen peroxide, ammonium persulfate, potassium persulfate, benzoyl peroxide, benzoyl tert-butyl peroxide One of the esters and methyl ethyl ketone peroxide.

上述的一种二元复配木质素基气凝胶吸附材料的制备方法,包括如下步骤:The preparation method of the above-mentioned binary compound lignin-based airgel adsorption material includes the following steps:

1)在20mL去离子水中入5.0-20.0wt%的丙烯酰胺、1.0-5.0wt%的交联剂、0-10.0wt%的羧基木聚糖、1.0-5.0wt%的木质素磺酸盐,并在室温下搅拌2h,然后向其中加入0.5-2.5wt%的引发剂和0.5-2.5wt%的四甲基乙二胺,搅拌均匀,然后将得到的溶液在室温下进一步聚合12h,得到水凝胶;1) Add 5.0-20.0wt% acrylamide, 1.0-5.0wt% cross-linking agent, 0-10.0wt% carboxyxylan, and 1.0-5.0wt% lignosulfonate into 20 mL deionized water. And stir at room temperature for 2h, then add 0.5-2.5wt% initiator and 0.5-2.5wt% tetramethylethylenediamine, stir evenly, and then further polymerize the resulting solution at room temperature for 12h to obtain water. gel;

2)用去离子水洗涤水凝胶,然后放入冷冻干燥机中,在-50℃下干燥48h后得二元复配木质素基气凝胶吸附材料。2) Wash the hydrogel with deionized water, then put it into a freeze dryer and dry it at -50°C for 48 hours to obtain a binary compound lignin-based airgel adsorption material.

上述任意一项所述的一种二元复配木质素基气凝胶吸附材料用于吸附印染废水中的亚甲基蓝。A binary compound lignin-based airgel adsorption material described in any one of the above is used to adsorb methylene blue in printing and dyeing wastewater.

进一步的,上述的应用,方法如下:调节亚甲基蓝溶液的pH值1-14,向其中加入二元复配木质素基气凝胶吸附材料进行吸附。Further, the above-mentioned application method is as follows: adjust the pH value of the methylene blue solution to 1-14, and add a binary compound lignin-based airgel adsorption material to it for adsorption.

更进一步的,上述的应用,所述亚甲基蓝溶液的浓度为10-200mg/mL,体积为50mL;二元复配木质素基气凝胶吸附材料的用量为0.01-0.09g。Furthermore, for the above application, the concentration of the methylene blue solution is 10-200 mg/mL and the volume is 50 mL; the dosage of the binary compound lignin-based airgel adsorption material is 0.01-0.09g.

更进一步的,上述的应用所述吸附的条件为:吸附温度为10-80℃,吸附时间为5-1440min。Furthermore, the conditions for the above-mentioned application of adsorption are: the adsorption temperature is 10-80°C, and the adsorption time is 5-1440 minutes.

本发明的有益效果是:The beneficial effects of the present invention are:

1、针对气凝胶材料成本高的问题,采用成本极低的工业废弃资源木质素磺酸盐,显著降低气凝胶材料的成本,带来了可观的经济效益。1. In view of the high cost of airgel materials, the extremely low-cost industrial waste resource lignosulfonate is used to significantly reduce the cost of airgel materials and bring considerable economic benefits.

2、针对传统气凝胶的有毒有害试剂使用问题,采用生物相容性好、可降解的生物质原料,可极大程度地避免生产过程对人体造成的危害及对环境造成的污染。2. In view of the problem of using toxic and harmful reagents in traditional aerogels, using biomass raw materials with good biocompatibility and degradability can greatly avoid harm to the human body and pollution to the environment during the production process.

3、针对传统气凝胶使用不可再生原料的问题,采用来源广泛的可再生有机碳材料,促进了碳资源的循环利用。3. In view of the problem of traditional aerogels using non-renewable raw materials, renewable organic carbon materials from a wide range of sources are used to promote the recycling of carbon resources.

4、针对单一木质素吸附效率有限的问题,向气凝胶中加入羧基木聚糖,使木质素磺酸盐和羧基木聚糖协同吸附,提高对亚甲基蓝的吸附效率。4. To address the problem of limited adsorption efficiency of single lignin, carboxyxylan was added to the aerogel to synergistically adsorb lignosulfonate and carboxyxylan to improve the adsorption efficiency of methylene blue.

5、针对现有木质素基气凝胶材料工艺复杂、操作不安全的问题,采用简单的溶液共混与冷冻干燥步骤,简化了合成工艺,操作安全性高。5. In order to solve the problems of complex process and unsafe operation of existing lignin-based aerogel materials, simple solution blending and freeze-drying steps are adopted to simplify the synthesis process and ensure high operational safety.

具体实施方式Detailed ways

下面结合实施例对本发明作进一步的详细说明,但本发明的实施方式不限于此。The present invention will be further described in detail below with reference to examples, but the implementation of the present invention is not limited thereto.

实施例1Example 1

将0.9900g木聚糖分散在9.00L 20%醇和水的混合溶液中,搅拌10分钟,然后在30℃下向其中加入4.93mL 25wt%的NaOH溶液,在搅拌30min后,向混合溶液中加入3.4900g氯乙酸钠,并在65℃下反应2小时;然后,再加入4.93mL 25wt%的NaOH溶液和3.4900g氯酸钠,在65℃下继续反应2小时。反应完成后,将得到的溶液用稀乙酸调节pH值至7,随后将混合溶液缓慢加入到乙醇中,此时在乙醇溶液中有沉淀生成,将得到的沉淀用95%乙醇洗涤三次,然后在50℃的烘箱中干燥48h,所得样品即为羧甲基木聚糖。Disperse 0.9900g xylan in 9.00L of a mixed solution of 20% alcohol and water, stir for 10 minutes, then add 4.93mL of 25wt% NaOH solution at 30°C, and after stirring for 30 minutes, add 3.4900 g of sodium chloroacetate, and react at 65°C for 2 hours; then, add 4.93mL of 25wt% NaOH solution and 3.4900g of sodium chlorate, and continue the reaction at 65°C for 2 hours. After the reaction is completed, the pH value of the obtained solution is adjusted to 7 with dilute acetic acid, and then the mixed solution is slowly added to ethanol. At this time, a precipitate is formed in the ethanol solution. The obtained precipitate is washed three times with 95% ethanol, and then After drying in an oven at 50°C for 48 hours, the obtained sample is carboxymethylxylan.

实施例2Example 2

在20mL去离子水中加入7.5wt%的丙烯酰胺、3.0wt%的N,N’-亚甲基双丙烯酰胺、10.0wt%的羧甲基木聚糖、5.0wt%的木质素磺酸钠,并在室温下搅拌2h,然后向其中加入1.5wt%的过硫酸铵和1.5wt%的四甲基乙二胺,搅拌均匀,水凝胶开始形成,然后将得到的溶液在室温下进一步聚合12h,得到水凝胶;用去离子水洗涤水凝胶,然后放入冷冻干燥机中,在-50℃下干燥48h后得二元复配木质素基气凝胶吸附材料。Add 7.5wt% acrylamide, 3.0wt% N,N'-methylenebisacrylamide, 10.0wt% carboxymethylxylan, and 5.0wt% sodium lignosulfonate to 20mL deionized water. And stir at room temperature for 2h, then add 1.5wt% ammonium persulfate and 1.5wt% tetramethylethylenediamine to it, stir evenly, the hydrogel begins to form, and then the resulting solution is further polymerized at room temperature for 12h. , to obtain a hydrogel; wash the hydrogel with deionized water, then put it into a freeze dryer, and dry it at -50°C for 48 hours to obtain a binary compound lignin-based airgel adsorption material.

取50mL浓度为50mg/L的亚甲基蓝溶液置于250mL的锥形瓶中,pH为6.9,然后加入0.0500g上述制备得到的二元复配木质素基气凝胶吸附材料,在室温下吸附24h,用紫外可见分光光度计检测其溶液中亚甲基蓝的吸光度,计算去除率和吸附量,去除率为28.45%,吸附量为13.34mg/g。Take 50 mL of methylene blue solution with a concentration of 50 mg/L and place it in a 250 mL Erlenmeyer flask with a pH of 6.9. Then add 0.0500 g of the binary compound lignin-based airgel adsorption material prepared above and adsorb at room temperature for 24 hours. Use a UV-visible spectrophotometer to detect the absorbance of methylene blue in the solution, and calculate the removal rate and adsorption capacity. The removal rate is 28.45% and the adsorption capacity is 13.34mg/g.

实施例3Example 3

在20mL去离子水中加入17.5wt%的丙烯酰胺、3.0wt%的N,N’-亚甲基双丙烯酰胺、10.0wt%的羧甲基木聚糖、5.0wt%的木质素磺酸钠,并在室温下搅拌2h,然后向其中加入1.5wt%的过硫酸铵和1.5wt%的四甲基乙二胺,搅拌均匀,水凝胶开始形成,然后将得到的溶液在室温下进一步聚合12h,得到水凝胶;用去离子水洗涤水凝胶,然后放入冷冻干燥机中,在-50℃下干燥48h后得二元复配木质素基气凝胶吸附材料。Add 17.5wt% acrylamide, 3.0wt% N,N'-methylenebisacrylamide, 10.0wt% carboxymethylxylan, and 5.0wt% sodium lignosulfonate to 20mL deionized water. And stir at room temperature for 2h, then add 1.5wt% ammonium persulfate and 1.5wt% tetramethylethylenediamine to it, stir evenly, the hydrogel begins to form, and then the resulting solution is further polymerized at room temperature for 12h. , to obtain a hydrogel; wash the hydrogel with deionized water, then put it into a freeze dryer, and dry it at -50°C for 48 hours to obtain a binary compound lignin-based airgel adsorption material.

取50mL浓度为50mg/L的亚甲基蓝溶液置于250mL的锥形瓶中,pH为6.9,然后加入0.0500g上述制备得到的二元复配木质素基气凝胶吸附材料,在室温下吸附24h,用紫外可见分光光度计检测其溶液中亚甲基蓝的吸光度,计算去除率和吸附量,去除率为24.06%,吸附量为11.16mg/g。Take 50 mL of methylene blue solution with a concentration of 50 mg/L and place it in a 250 mL Erlenmeyer flask with a pH of 6.9. Then add 0.0500 g of the binary compound lignin-based airgel adsorption material prepared above and adsorb at room temperature for 24 hours. Use a UV-visible spectrophotometer to detect the absorbance of methylene blue in the solution, and calculate the removal rate and adsorption capacity. The removal rate is 24.06% and the adsorption capacity is 11.16mg/g.

实施例4Example 4

在20mL去离子水中加入10.0wt%的丙烯酰胺、2.0wt%的N,N’-亚甲基双丙烯酰胺、10.0wt%的羧甲基木聚糖、5.0wt%的木质素磺酸钠,并在室温下搅拌2h,然后向其中加入1.5wt%的过硫酸铵和1.5wt%的四甲基乙二胺,搅拌均匀,水凝胶开始形成,然后将得到的溶液在室温下进一步聚合12h,得到水凝胶;用去离子水洗涤水凝胶,然后放入冷冻干燥机中,在-50℃下干燥48h后得二元复配木质素基气凝胶吸附材料。Add 10.0wt% acrylamide, 2.0wt% N,N'-methylenebisacrylamide, 10.0wt% carboxymethylxylan, and 5.0wt% sodium lignosulfonate to 20mL deionized water. And stir at room temperature for 2h, then add 1.5wt% ammonium persulfate and 1.5wt% tetramethylethylenediamine to it, stir evenly, the hydrogel begins to form, and then the resulting solution is further polymerized at room temperature for 12h. , to obtain a hydrogel; wash the hydrogel with deionized water, then put it into a freeze dryer, and dry it at -50°C for 48 hours to obtain a binary compound lignin-based airgel adsorption material.

取50mL浓度为50mg/L的亚甲基蓝溶液置于250mL的锥形瓶中,pH为6.9,然后加入0.0500g上述制备得到的二元复配木质素基气凝胶吸附材料,在室温下吸附24h,用紫外可见分光光度计检测其溶液中亚甲基蓝的吸光度,计算去除率和吸附量,去除率为3.14%,吸附量为1.35mg/g。Take 50 mL of methylene blue solution with a concentration of 50 mg/L and place it in a 250 mL Erlenmeyer flask with a pH of 6.9. Then add 0.0500 g of the binary compound lignin-based airgel adsorption material prepared above and adsorb at room temperature for 24 hours. Use a UV-visible spectrophotometer to detect the absorbance of methylene blue in the solution, and calculate the removal rate and adsorption capacity. The removal rate is 3.14% and the adsorption capacity is 1.35 mg/g.

实施例5Example 5

在20mL去离子水中加入10.0wt%的丙烯酰胺、5.0wt%的N,N’-亚甲基双丙烯酰胺、10.0wt%的羧甲基木聚糖、5.0wt%的木质素磺酸钠,并在室温下搅拌2h,然后向其中加入1.5wt%的过硫酸铵和1.5wt%的四甲基乙二胺,搅拌均匀,水凝胶开始形成,然后将得到的溶液在室温下进一步聚合12h,得到水凝胶;用去离子水洗涤水凝胶,然后放入冷冻干燥机中,在-50℃下干燥48h后得二元复配木质素基气凝胶吸附材料。Add 10.0wt% acrylamide, 5.0wt% N,N'-methylenebisacrylamide, 10.0wt% carboxymethylxylan, and 5.0wt% sodium lignosulfonate to 20mL deionized water. And stir at room temperature for 2h, then add 1.5wt% ammonium persulfate and 1.5wt% tetramethylethylenediamine to it, stir evenly, the hydrogel begins to form, and then the resulting solution is further polymerized at room temperature for 12h. , to obtain a hydrogel; wash the hydrogel with deionized water, then put it into a freeze dryer, and dry it at -50°C for 48 hours to obtain a binary compound lignin-based airgel adsorption material.

取50mL浓度为50mg/L的亚甲基蓝溶液置于250mL的锥形瓶中,pH为6.9,然后加入0.0500g上述制备得到的二元复配木质素基气凝胶吸附材料,在室温下吸附24h,用紫外可见分光光度计检测其溶液中亚甲基蓝的吸光度,计算去除率和吸附量,去除率为30.40%,吸附量为13.64mg/g。Take 50 mL of methylene blue solution with a concentration of 50 mg/L and place it in a 250 mL Erlenmeyer flask with a pH of 6.9. Then add 0.0500 g of the binary compound lignin-based airgel adsorption material prepared above and adsorb at room temperature for 24 hours. Use a UV-visible spectrophotometer to detect the absorbance of methylene blue in the solution, and calculate the removal rate and adsorption capacity. The removal rate is 30.40% and the adsorption capacity is 13.64mg/g.

实施例6Example 6

在20mL去离子水中加入10.0wt%的丙烯酰胺、5.0wt%的N,N’-亚甲基双丙烯酰胺、10.0wt%的羧甲基木聚糖、5.0wt%的木质素磺酸钠,并在室温下搅拌2h,然后向其中加入1.0wt%的过硫酸铵和1.5wt%的四甲基乙二胺,搅拌均匀,水凝胶开始形成,然后将得到的溶液在室温下进一步聚合12h,得到水凝胶;用去离子水洗涤水凝胶,然后放入冷冻干燥机中,在-50℃下干燥48h后得二元复配木质素基气凝胶吸附材料。Add 10.0wt% acrylamide, 5.0wt% N,N'-methylenebisacrylamide, 10.0wt% carboxymethylxylan, and 5.0wt% sodium lignosulfonate to 20mL deionized water. And stir at room temperature for 2h, then add 1.0wt% ammonium persulfate and 1.5wt% tetramethylethylenediamine to it, stir evenly, the hydrogel begins to form, and then the resulting solution is further polymerized at room temperature for 12h. , to obtain a hydrogel; wash the hydrogel with deionized water, then put it into a freeze dryer, and dry it at -50°C for 48 hours to obtain a binary compound lignin-based airgel adsorption material.

取50mL浓度为50mg/L的亚甲基蓝溶液置于250mL的锥形瓶中,pH为6.9,然后加入0.0500g上述制备得到的二元复配木质素基气凝胶吸附材料,在室温下吸附24h,用紫外可见分光光度计检测其溶液中亚甲基蓝的吸光度,计算去除率和吸附量,去除率为54.10%,吸附量为28.59mg/g。Take 50 mL of methylene blue solution with a concentration of 50 mg/L and place it in a 250 mL Erlenmeyer flask with a pH of 6.9. Then add 0.0500 g of the binary compound lignin-based airgel adsorption material prepared above and adsorb at room temperature for 24 hours. Use a UV-visible spectrophotometer to detect the absorbance of methylene blue in the solution, and calculate the removal rate and adsorption capacity. The removal rate is 54.10% and the adsorption capacity is 28.59mg/g.

实施例7Example 7

在20mL去离子水中加入10.0wt%的丙烯酰胺、5.0wt%的N,N’-亚甲基双丙烯酰胺、10.0wt%的羧甲基木聚糖、5.0wt%的木质素磺酸钠,并在室温下搅拌2h,然后向其中加入2.5wt%的过硫酸铵和1.5wt%的四甲基乙二胺,搅拌均匀,水凝胶开始形成,然后将得到的溶液在室温下进一步聚合12h,得到水凝胶;用去离子水洗涤水凝胶,然后放入冷冻干燥机中,在-50℃下干燥48h后得二元复配木质素基气凝胶吸附材料。Add 10.0wt% acrylamide, 5.0wt% N,N'-methylenebisacrylamide, 10.0wt% carboxymethylxylan, and 5.0wt% sodium lignosulfonate to 20mL deionized water. And stir at room temperature for 2h, then add 2.5wt% ammonium persulfate and 1.5wt% tetramethylethylenediamine to it, stir evenly, the hydrogel begins to form, and then the resulting solution is further polymerized at room temperature for 12h. , to obtain a hydrogel; wash the hydrogel with deionized water, then put it into a freeze dryer, and dry it at -50°C for 48 hours to obtain a binary compound lignin-based airgel adsorption material.

取50mL浓度为50mg/L的亚甲基蓝溶液置于250mL的锥形瓶中,pH为6.9,然后加入0.0500g上述制备得到的二元复配木质素基气凝胶吸附材料,在室温下吸附24h,用紫外可见分光光度计检测其溶液中亚甲基蓝的吸光度,计算去除率和吸附量,去除率为27.61%,吸附量为14.20mg/g。Take 50 mL of methylene blue solution with a concentration of 50 mg/L and place it in a 250 mL Erlenmeyer flask with a pH of 6.9. Then add 0.0500 g of the binary compound lignin-based airgel adsorption material prepared above and adsorb at room temperature for 24 hours. Use a UV-visible spectrophotometer to detect the absorbance of methylene blue in the solution, and calculate the removal rate and adsorption capacity. The removal rate is 27.61% and the adsorption capacity is 14.20 mg/g.

实施例8Example 8

在20mL去离子水中加入10.0wt%的丙烯酰胺、5.0wt%的N,N’-亚甲基双丙烯酰胺、5.0wt%的羧甲基木聚糖、5.0wt%的木质素磺酸钠,并在室温下搅拌2h,然后向其中加入1.5wt%的过硫酸铵和1.5wt%的四甲基乙二胺,搅拌均匀,水凝胶开始形成,然后将得到的溶液在室温下进一步聚合12h,得到水凝胶;用去离子水洗涤水凝胶,然后放入冷冻干燥机中,在-50℃下干燥48h后得二元复配木质素基气凝胶吸附材料。Add 10.0wt% acrylamide, 5.0wt% N,N'-methylenebisacrylamide, 5.0wt% carboxymethylxylan, and 5.0wt% sodium lignosulfonate to 20mL deionized water. And stir at room temperature for 2h, then add 1.5wt% ammonium persulfate and 1.5wt% tetramethylethylenediamine to it, stir evenly, the hydrogel begins to form, and then the resulting solution is further polymerized at room temperature for 12h. , to obtain a hydrogel; wash the hydrogel with deionized water, then put it into a freeze dryer, and dry it at -50°C for 48 hours to obtain a binary compound lignin-based airgel adsorption material.

取50mL浓度为50mg/L的亚甲基蓝溶液置于250mL的锥形瓶中,pH为6.9,然后加入0.0500g上述制备得到的二元复配木质素基气凝胶吸附材料,在室温下吸附24h,用紫外可见分光光度计检测其溶液中亚甲基蓝的吸光度,计算去除率和吸附量,去除率为31.54%,吸附量为15.19mg/g。Take 50 mL of methylene blue solution with a concentration of 50 mg/L and place it in a 250 mL Erlenmeyer flask with a pH of 6.9. Then add 0.0500 g of the binary compound lignin-based airgel adsorption material prepared above and adsorb at room temperature for 24 hours. Use a UV-visible spectrophotometer to detect the absorbance of methylene blue in the solution, and calculate the removal rate and adsorption capacity. The removal rate is 31.54% and the adsorption capacity is 15.19mg/g.

实施例9Example 9

在20mL去离子水中加入10.0wt%的丙烯酰胺、5.0wt%的N,N’-亚甲基双丙烯酰胺、10.0wt%的羧甲基木聚糖、1.0wt%的木质素磺酸钠,并在室温下搅拌2h,然后向其中加入1.5wt%的过硫酸铵和1.5wt%的四甲基乙二胺,搅拌均匀,水凝胶开始形成,然后将得到的溶液在室温下进一步聚合12h,得到水凝胶;用去离子水洗涤水凝胶,然后放入冷冻干燥机中,在-50℃下干燥48h后得二元复配木质素基气凝胶吸附材料。Add 10.0wt% acrylamide, 5.0wt% N,N'-methylenebisacrylamide, 10.0wt% carboxymethylxylan, and 1.0wt% sodium lignosulfonate to 20mL deionized water. And stir at room temperature for 2h, then add 1.5wt% ammonium persulfate and 1.5wt% tetramethylethylenediamine to it, stir evenly, the hydrogel begins to form, and then the resulting solution is further polymerized at room temperature for 12h. , to obtain a hydrogel; wash the hydrogel with deionized water, then put it into a freeze dryer, and dry it at -50°C for 48 hours to obtain a binary compound lignin-based airgel adsorption material.

取50mL浓度为50mg/L的亚甲基蓝溶液置于250mL的锥形瓶中,pH为6.9,然后加入0.0500g上述制备得到的二元复配木质素基气凝胶吸附材料,在室温下吸附24h,用紫外可见分光光度计检测其溶液中亚甲基蓝的吸光度,计算去除率和吸附量,去除率为16.56%,吸附量为8.07mg/g。Take 50 mL of methylene blue solution with a concentration of 50 mg/L and place it in a 250 mL Erlenmeyer flask with a pH of 6.9. Then add 0.0500 g of the binary compound lignin-based airgel adsorption material prepared above and adsorb at room temperature for 24 hours. Use a UV-visible spectrophotometer to detect the absorbance of methylene blue in the solution, and calculate the removal rate and adsorption capacity. The removal rate is 16.56% and the adsorption capacity is 8.07mg/g.

实施例10Example 10

在20mL去离子水中加入10.0wt%的丙烯酰胺、5.0wt%的N,N’-亚甲基双丙烯酰胺、8.0wt%的羧甲基木聚糖、4.0wt%的木质素磺酸钠,并在室温下搅拌2h,然后向其中加入1.5wt%的过硫酸铵和1.5wt%的四甲基乙二胺,搅拌均匀,水凝胶开始形成,然后将得到的溶液在室温下进一步聚合12h,得到水凝胶;用去离子水洗涤水凝胶,然后放入冷冻干燥机中,在-50℃下干燥48h后得二元复配木质素基气凝胶吸附材料。Add 10.0wt% acrylamide, 5.0wt% N,N'-methylenebisacrylamide, 8.0wt% carboxymethylxylan, and 4.0wt% sodium lignosulfonate to 20mL deionized water. And stir at room temperature for 2h, then add 1.5wt% ammonium persulfate and 1.5wt% tetramethylethylenediamine to it, stir evenly, the hydrogel begins to form, and then the resulting solution is further polymerized at room temperature for 12h. , to obtain a hydrogel; wash the hydrogel with deionized water, then put it into a freeze dryer, and dry it at -50°C for 48 hours to obtain a binary compound lignin-based airgel adsorption material.

取50mL浓度为50mg/L的亚甲基蓝溶液置于250mL的锥形瓶中,调节pH为3,然后加入0.0500g上述制备得到的二元复配木质素基气凝胶吸附材料,在室温下吸附24h,用紫外可见分光光度计检测其溶液中亚甲基蓝的吸光度,计算去除率和吸附量,去除率为19.48%,吸附量为9.74mg/g。Take 50 mL of methylene blue solution with a concentration of 50 mg/L and place it in a 250 mL Erlenmeyer flask, adjust the pH to 3, then add 0.0500 g of the binary compound lignin-based airgel adsorption material prepared above, and adsorb at room temperature for 24 hours. , use a UV-visible spectrophotometer to detect the absorbance of methylene blue in the solution, and calculate the removal rate and adsorption capacity. The removal rate is 19.48% and the adsorption capacity is 9.74mg/g.

实施例11Example 11

在20mL去离子水中加入10.0wt%的丙烯酰胺、5.0wt%的N,N’-亚甲基双丙烯酰胺、8.0wt%的羧甲基木聚糖、4.0wt%的木质素磺酸钠,并在室温下搅拌2h,然后向其中加入1.5wt%的过硫酸铵和1.5wt%的四甲基乙二胺,搅拌均匀,水凝胶开始形成,然后将得到的溶液在室温下进一步聚合12h,得到水凝胶;用去离子水洗涤水凝胶,然后放入冷冻干燥机中,在-50℃下干燥48h后得二元复配木质素基气凝胶吸附材料。Add 10.0wt% acrylamide, 5.0wt% N,N'-methylenebisacrylamide, 8.0wt% carboxymethylxylan, and 4.0wt% sodium lignosulfonate to 20mL deionized water. And stir at room temperature for 2h, then add 1.5wt% ammonium persulfate and 1.5wt% tetramethylethylenediamine to it, stir evenly, the hydrogel begins to form, and then the resulting solution is further polymerized at room temperature for 12h. , to obtain a hydrogel; wash the hydrogel with deionized water, then put it into a freeze dryer, and dry it at -50°C for 48 hours to obtain a binary compound lignin-based airgel adsorption material.

取50mL浓度为50mg/L的亚甲基蓝溶液置于250mL的锥形瓶中,调节pH为11,然后加入0.0500g上述制备得到的二元复配木质素基气凝胶吸附材料,在室温下吸附24h,用紫外可见分光光度计检测其溶液中亚甲基蓝的吸光度,计算去除率和吸附量,去除率为40.22%,吸附量为17.80mg/g。Take 50 mL of methylene blue solution with a concentration of 50 mg/L and place it in a 250 mL Erlenmeyer flask, adjust the pH to 11, then add 0.0500 g of the binary compound lignin-based airgel adsorption material prepared above, and adsorb at room temperature for 24 hours. , use a UV-visible spectrophotometer to detect the absorbance of methylene blue in the solution, and calculate the removal rate and adsorption capacity. The removal rate is 40.22% and the adsorption capacity is 17.80mg/g.

实施例12Example 12

在20mL去离子水中加入10.0wt%的丙烯酰胺、5.0wt%的N,N’-亚甲基双丙烯酰胺、8.0wt%的羧甲基木聚糖、4.0wt%的木质素磺酸钠,并在室温下搅拌2h,然后向其中加入1.5wt%的过硫酸铵和1.5wt%的四甲基乙二胺,搅拌均匀,水凝胶开始形成,然后将得到的溶液在室温下进一步聚合12h,得到水凝胶;用去离子水洗涤水凝胶,然后放入冷冻干燥机中,在-50℃下干燥48h后得二元复配木质素基气凝胶吸附材料。Add 10.0wt% acrylamide, 5.0wt% N,N'-methylenebisacrylamide, 8.0wt% carboxymethylxylan, and 4.0wt% sodium lignosulfonate to 20mL deionized water. And stir at room temperature for 2h, then add 1.5wt% ammonium persulfate and 1.5wt% tetramethylethylenediamine to it, stir evenly, the hydrogel begins to form, and then the resulting solution is further polymerized at room temperature for 12h. , to obtain a hydrogel; wash the hydrogel with deionized water, then put it into a freeze dryer, and dry it at -50°C for 48 hours to obtain a binary compound lignin-based airgel adsorption material.

取50mL浓度为50mg/L的亚甲基蓝溶液置于250mL的锥形瓶中,调节pH为11,然后加入0.0500g上述制备得到的二元复配木质素基气凝胶吸附材料,在室温下吸附15min,用紫外可见分光光度计检测其溶液中亚甲基蓝的吸光度,计算去除率和吸附量,去除率为4.06%,吸附量为3.87mg/g。Take 50 mL of methylene blue solution with a concentration of 50 mg/L and place it in a 250 mL Erlenmeyer flask, adjust the pH to 11, then add 0.0500 g of the binary compound lignin-based airgel adsorption material prepared above, and adsorb at room temperature for 15 minutes. , use a UV-visible spectrophotometer to detect the absorbance of methylene blue in the solution, and calculate the removal rate and adsorption capacity. The removal rate is 4.06% and the adsorption capacity is 3.87mg/g.

实施例13Example 13

在20mL去离子水中加入10.0wt%的丙烯酰胺、5.0wt%的N,N’-亚甲基双丙烯酰胺、8.0wt%的羧甲基木聚糖、4.0wt%的木质素磺酸钠,并在室温下搅拌2h,然后向其中加入1.5wt%的过硫酸铵和1.5wt%的四甲基乙二胺,搅拌均匀,水凝胶开始形成,然后将得到的溶液在室温下进一步聚合12h,得到水凝胶;用去离子水洗涤水凝胶,然后放入冷冻干燥机中,在-50℃下干燥48h后得二元复配木质素基气凝胶吸附材料。Add 10.0wt% acrylamide, 5.0wt% N,N'-methylenebisacrylamide, 8.0wt% carboxymethylxylan, and 4.0wt% sodium lignosulfonate to 20mL deionized water. And stir at room temperature for 2h, then add 1.5wt% ammonium persulfate and 1.5wt% tetramethylethylenediamine to it, stir evenly, the hydrogel begins to form, and then the resulting solution is further polymerized at room temperature for 12h. , to obtain a hydrogel; wash the hydrogel with deionized water, then put it into a freeze dryer, and dry it at -50°C for 48 hours to obtain a binary compound lignin-based airgel adsorption material.

取50mL浓度为50mg/L的亚甲基蓝溶液置于250mL的锥形瓶中,调节pH为11,然后加入0.0500g上述制备得到的二元复配木质素基气凝胶吸附材料,在室温下吸附720min,用紫外可见分光光度计检测其溶液中亚甲基蓝的吸光度,计算去除率和吸附量,去除率为17.38%,吸附量为26.83mg/g。Take 50 mL of methylene blue solution with a concentration of 50 mg/L and place it in a 250 mL Erlenmeyer flask, adjust the pH to 11, then add 0.0500 g of the binary compound lignin-based airgel adsorption material prepared above, and adsorb at room temperature for 720 minutes. , use a UV-visible spectrophotometer to detect the absorbance of methylene blue in the solution, and calculate the removal rate and adsorption capacity. The removal rate is 17.38% and the adsorption capacity is 26.83mg/g.

实施例14Example 14

在20mL去离子水中加入10.0wt%的丙烯酰胺、5.0wt%的N,N’-亚甲基双丙烯酰胺、8.0wt%的羧甲基木聚糖、4.0wt%的木质素磺酸钠,并在室温下搅拌2h,然后向其中加入1.5wt%的过硫酸铵和1.5wt%的四甲基乙二胺,搅拌均匀,水凝胶开始形成,然后将得到的溶液在室温下进一步聚合12h,得到水凝胶;用去离子水洗涤水凝胶,然后放入冷冻干燥机中,在-50℃下干燥48h后得二元复配木质素基气凝胶吸附材料。Add 10.0wt% acrylamide, 5.0wt% N,N'-methylenebisacrylamide, 8.0wt% carboxymethylxylan, and 4.0wt% sodium lignosulfonate to 20mL deionized water. And stir at room temperature for 2h, then add 1.5wt% ammonium persulfate and 1.5wt% tetramethylethylenediamine to it, stir evenly, the hydrogel begins to form, and then the resulting solution is further polymerized at room temperature for 12h. , to obtain a hydrogel; wash the hydrogel with deionized water, then put it into a freeze dryer, and dry it at -50°C for 48 hours to obtain a binary compound lignin-based airgel adsorption material.

取50mL浓度为50mg/L的亚甲基蓝溶液置于250mL的锥形瓶中,调节pH为11,然后加入0.0100g上述制备得到的二元复配木质素基气凝胶吸附材料,在室温下吸附720min,用紫外可见分光光度计检测其溶液中亚甲基蓝的吸光度,计算去除率和吸附量,去除率为15.94%,吸附量为38.31mg/g。Take 50 mL of methylene blue solution with a concentration of 50 mg/L and place it in a 250 mL Erlenmeyer flask, adjust the pH to 11, then add 0.0100 g of the binary compound lignin-based airgel adsorption material prepared above, and adsorb at room temperature for 720 minutes. , use a UV-visible spectrophotometer to detect the absorbance of methylene blue in the solution, and calculate the removal rate and adsorption capacity. The removal rate is 15.94% and the adsorption capacity is 38.31mg/g.

实施例15Example 15

在20mL去离子水中加入10.0wt%的丙烯酰胺、5.0wt%的N,N’-亚甲基双丙烯酰胺、8.0wt%的羧甲基木聚糖、4.0wt%的木质素磺酸钠,并在室温下搅拌2h,然后向其中加入1.5wt%的过硫酸铵和1.5wt%的四甲基乙二胺,搅拌均匀,水凝胶开始形成,然后将得到的溶液在室温下进一步聚合12h,得到水凝胶;用去离子水洗涤水凝胶,然后放入冷冻干燥机中,在-50℃下干燥48h后得二元复配木质素基气凝胶吸附材料。Add 10.0wt% acrylamide, 5.0wt% N,N'-methylenebisacrylamide, 8.0wt% carboxymethylxylan, and 4.0wt% sodium lignosulfonate to 20mL deionized water. And stir at room temperature for 2h, then add 1.5wt% ammonium persulfate and 1.5wt% tetramethylethylenediamine to it, stir evenly, the hydrogel begins to form, and then the resulting solution is further polymerized at room temperature for 12h. , to obtain a hydrogel; wash the hydrogel with deionized water, then put it into a freeze dryer, and dry it at -50°C for 48 hours to obtain a binary compound lignin-based airgel adsorption material.

取50mL浓度为50mg/L的亚甲基蓝溶液置于250mL的锥形瓶中,调节pH为11,然后加入0.0900g上述制备得到的二元复配木质素基气凝胶吸附材料,在室温下吸附720min,用紫外可见分光光度计检测其溶液中亚甲基蓝的吸光度,计算去除率和吸附量,去除率为28.96%,吸附量为7.95mg/g。Take 50 mL of methylene blue solution with a concentration of 50 mg/L and place it in a 250 mL Erlenmeyer flask, adjust the pH to 11, then add 0.0900 g of the binary compound lignin-based airgel adsorption material prepared above, and adsorb at room temperature for 720 minutes. , use a UV-visible spectrophotometer to detect the absorbance of methylene blue in the solution, and calculate the removal rate and adsorption capacity. The removal rate is 28.96% and the adsorption capacity is 7.95mg/g.

实施例16Example 16

在20mL去离子水中加入10.0wt%的丙烯酰胺、5.0wt%的N,N’-亚甲基双丙烯酰胺、8.0wt%的羧甲基木聚糖、4.0wt%的木质素磺酸钠,并在室温下搅拌2h,然后向其中加入1.5wt%的过硫酸铵和1.5wt%的四甲基乙二胺,搅拌均匀,水凝胶开始形成,然后将得到的溶液在室温下进一步聚合12h,得到水凝胶;用去离子水洗涤水凝胶,然后放入冷冻干燥机中,在-50℃下干燥48h后得二元复配木质素基气凝胶吸附材料。Add 10.0wt% acrylamide, 5.0wt% N,N'-methylenebisacrylamide, 8.0wt% carboxymethylxylan, and 4.0wt% sodium lignosulfonate to 20mL deionized water. And stir at room temperature for 2h, then add 1.5wt% ammonium persulfate and 1.5wt% tetramethylethylenediamine to it, stir evenly, the hydrogel begins to form, and then the resulting solution is further polymerized at room temperature for 12h. , to obtain a hydrogel; wash the hydrogel with deionized water, then put it into a freeze dryer, and dry it at -50°C for 48 hours to obtain a binary compound lignin-based airgel adsorption material.

取50mL浓度为10mg/L的亚甲基蓝溶液置于250mL的锥形瓶中,调节pH为11,然后加入0.0500g上述制备得到的二元复配木质素基气凝胶吸附材料,在室温下吸附720min,用紫外可见分光光度计检测其溶液中亚甲基蓝的吸光度,计算去除率和吸附量,去除率为34.38%,吸附量为5.87mg/g。Take 50 mL of methylene blue solution with a concentration of 10 mg/L and place it in a 250 mL Erlenmeyer flask, adjust the pH to 11, then add 0.0500 g of the binary compound lignin-based airgel adsorption material prepared above, and adsorb at room temperature for 720 minutes. , use a UV-visible spectrophotometer to detect the absorbance of methylene blue in the solution, and calculate the removal rate and adsorption capacity. The removal rate is 34.38%, and the adsorption capacity is 5.87mg/g.

实施例17Example 17

在20mL去离子水中加入10.0wt%的丙烯酰胺、5.0wt%的N,N’-亚甲基双丙烯酰胺、8.0wt%的羧甲基木聚糖、4.0wt%的木质素磺酸钠,并在室温下搅拌2h,然后向其中加入1.5wt%的过硫酸铵和1.5wt%的四甲基乙二胺,搅拌均匀,水凝胶开始形成,然后将得到的溶液在室温下进一步聚合12h,得到水凝胶;用去离子水洗涤水凝胶,然后放入冷冻干燥机中,在-50℃下干燥48h后得二元复配木质素基气凝胶吸附材料。Add 10.0wt% acrylamide, 5.0wt% N,N'-methylenebisacrylamide, 8.0wt% carboxymethylxylan, and 4.0wt% sodium lignosulfonate to 20mL deionized water. And stir at room temperature for 2h, then add 1.5wt% ammonium persulfate and 1.5wt% tetramethylethylenediamine to it, stir evenly, the hydrogel begins to form, and then the resulting solution is further polymerized at room temperature for 12h. , to obtain a hydrogel; wash the hydrogel with deionized water, then put it into a freeze dryer, and dry it at -50°C for 48 hours to obtain a binary compound lignin-based airgel adsorption material.

取50mL浓度为200mg/L的亚甲基蓝溶液置于250mL的锥形瓶中,调节pH为11,然后加入0.0500g上述制备得到的二元复配木质素基气凝胶吸附材料,在室温下吸附720min,用紫外可见分光光度计检测其溶液中亚甲基蓝的吸光度,计算去除率和吸附量,去除率为8.34%,吸附量为30.34mg/g。Take 50 mL of methylene blue solution with a concentration of 200 mg/L and place it in a 250 mL Erlenmeyer flask, adjust the pH to 11, then add 0.0500 g of the binary compound lignin-based airgel adsorption material prepared above, and adsorb at room temperature for 720 minutes. , use a UV-visible spectrophotometer to detect the absorbance of methylene blue in the solution, and calculate the removal rate and adsorption capacity. The removal rate is 8.34% and the adsorption capacity is 30.34mg/g.

实施例18Example 18

在20mL去离子水中加入10.0wt%的丙烯酰胺、5.0wt%的N,N’-亚甲基双丙烯酰胺、8.0wt%的羧甲基木聚糖、4.0wt%的木质素磺酸钠,并在室温下搅拌2h,然后向其中加入1.5wt%的过硫酸铵和1.5wt%的四甲基乙二胺,搅拌均匀,水凝胶开始形成,然后将得到的溶液在室温下进一步聚合12h,得到水凝胶;用去离子水洗涤水凝胶,然后放入冷冻干燥机中,在-50℃下干燥48h后得二元复配木质素基气凝胶吸附材料。Add 10.0wt% acrylamide, 5.0wt% N,N'-methylenebisacrylamide, 8.0wt% carboxymethylxylan, and 4.0wt% sodium lignosulfonate to 20mL deionized water. And stir at room temperature for 2h, then add 1.5wt% ammonium persulfate and 1.5wt% tetramethylethylenediamine to it, stir evenly, the hydrogel begins to form, and then the resulting solution is further polymerized at room temperature for 12h. , to obtain a hydrogel; wash the hydrogel with deionized water, then put it into a freeze dryer, and dry it at -50°C for 48 hours to obtain a binary compound lignin-based airgel adsorption material.

取50mL浓度为50mg/L的亚甲基蓝溶液置于250mL的锥形瓶中,调节pH为11,然后加入0.0500g上述制备得到的二元复配木质素基气凝胶吸附材料,在20℃下吸附720min,用紫外可见分光光度计检测其溶液中亚甲基蓝的吸光度,计算去除率和吸附量,去除率为31.32%,吸附量为24.77mg/g。Take 50 mL of methylene blue solution with a concentration of 50 mg/L and place it in a 250 mL Erlenmeyer flask, adjust the pH to 11, then add 0.0500 g of the binary compound lignin-based airgel adsorption material prepared above, and adsorb at 20°C. At 720 minutes, use a UV-visible spectrophotometer to detect the absorbance of methylene blue in the solution, and calculate the removal rate and adsorption capacity. The removal rate is 31.32% and the adsorption capacity is 24.77mg/g.

实施例19Example 19

在20mL去离子水中加入10.0wt%的丙烯酰胺、5.0wt%的N,N’-亚甲基双丙烯酰胺、8.0wt%的羧甲基木聚糖、4.0wt%的木质素磺酸钠,并在室温下搅拌2h,然后向其中加入1.5wt%的过硫酸铵和1.5wt%的四甲基乙二胺,搅拌均匀,水凝胶开始形成,然后将得到的溶液在室温下进一步聚合12h,得到水凝胶;用去离子水洗涤水凝胶,然后放入冷冻干燥机中,在-50℃下干燥48h后得二元复配木质素基气凝胶吸附材料。Add 10.0wt% acrylamide, 5.0wt% N,N'-methylenebisacrylamide, 8.0wt% carboxymethylxylan, and 4.0wt% sodium lignosulfonate to 20mL deionized water. And stir at room temperature for 2h, then add 1.5wt% ammonium persulfate and 1.5wt% tetramethylethylenediamine to it, stir evenly, the hydrogel begins to form, and then the resulting solution is further polymerized at room temperature for 12h. , to obtain a hydrogel; wash the hydrogel with deionized water, then put it into a freeze dryer, and dry it at -50°C for 48 hours to obtain a binary compound lignin-based airgel adsorption material.

取50mL浓度为50mg/L的亚甲基蓝溶液置于250mL的锥形瓶中,调节pH为11,然后加入0.0500g上述制备得到的二元复配木质素基气凝胶吸附材料,在40℃下吸附720min,用紫外可见分光光度计检测其溶液中亚甲基蓝的吸光度,计算去除率和吸附量,去除率为51.11%,吸附量为39.80mg/g。Take 50 mL of methylene blue solution with a concentration of 50 mg/L and place it in a 250 mL Erlenmeyer flask, adjust the pH to 11, then add 0.0500 g of the binary compound lignin-based airgel adsorption material prepared above, and adsorb at 40°C. 720min, use a UV-visible spectrophotometer to detect the absorbance of methylene blue in the solution, and calculate the removal rate and adsorption capacity. The removal rate is 51.11%, and the adsorption capacity is 39.80mg/g.

以上为对本发明做的示例性描述,在不脱离本发明核心情况下,任何简单的变形、修饰、替代、组合、简化,均为等效的替换方式,都包含在本发明的保护范围之内。The above is an exemplary description of the present invention. Without departing from the core of the present invention, any simple transformation, modification, replacement, combination, and simplification are all equivalent replacements and are included in the protection scope of the present invention. .

Claims (10)

1.一种二元复配木质素基气凝胶吸附材料,其特征在于,所述的二元复配木质素基气凝胶吸附材料由1.0-5.0wt%的木质素磺酸盐、0-10.0wt%的羧基木聚糖、5.0-20.0wt%的丙烯酰胺、1.0-5.0wt%的交联剂、0.5-2.5wt%的引发剂及0.5-2.5wt%的四甲基乙二胺反应制成。1. A binary compound lignin-based airgel adsorbent material, characterized in that the binary compound lignin-based airgel adsorbent material is composed of 1.0-5.0wt% lignin sulfonate, 0 -10.0wt% carboxyxylan, 5.0-20.0wt% acrylamide, 1.0-5.0wt% cross-linking agent, 0.5-2.5wt% initiator and 0.5-2.5wt% tetramethylethylenediamine Made by reaction. 2.根据权利要求1所述的一种二元复配木质素基气凝胶吸附材料,其特征在于,所述木质素磺酸盐为木质素磺酸钠和木质素磺酸钙中的一种或两种的组合。2. A binary compound lignin-based airgel adsorbent material according to claim 1, characterized in that the lignosulfonate is one of sodium lignosulfonate and calcium lignosulfonate. one or a combination of two. 3.根据权利要求1所述的一种二元复配木质素基气凝胶吸附材料,其特征在于,所述羧基木聚糖为羧甲基木聚糖或羧乙基木聚糖。3. A binary compound lignin-based airgel adsorption material according to claim 1, characterized in that the carboxyxylan is carboxymethylxylan or carboxyethylxylan. 4.根据权利要求1所述的一种二元复配木质素基气凝胶吸附材料,其特征在于,所述交联剂为N,N’-亚甲基双丙烯酰胺或氢氧化铝。4. A binary compound lignin-based airgel adsorbent material according to claim 1, characterized in that the cross-linking agent is N, N'-methylene bisacrylamide or aluminum hydroxide. 5.根据权利要求1所述的一种二元复配木质素基气凝胶吸附材料,其特征在于,所述引发剂为过氧化氢、过硫酸铵、过硫酸钾、过氧化苯甲酰、过氧化苯甲酰叔丁酯和过氧化甲乙酮中的一种。5. A kind of binary composite lignin-based airgel adsorbent material according to claim 1, characterized in that the initiator is hydrogen peroxide, ammonium persulfate, potassium persulfate, benzoyl peroxide , one of benzoyl tert-butyl peroxide and methyl ethyl ketone peroxide. 6.权利要求1所述的一种二元复配木质素基气凝胶吸附材料的制备方法,其特征在于,包括如下步骤:6. The preparation method of a binary compound lignin-based airgel adsorbent material according to claim 1, characterized in that it includes the following steps: 1)在20mL去离子水中入5.0-20.0wt%的丙烯酰胺、1.0-5.0wt%的交联剂、0-10.0wt%的羧基木聚糖、1.0-5.0wt%的木质素磺酸盐,并在室温下搅拌2h,然后向其中加入0.5-2.5wt%的引发剂和0.5-2.5wt%的四甲基乙二胺,搅拌均匀,然后将得到的溶液在室温下进一步聚合12h,得到水凝胶;1) Add 5.0-20.0wt% acrylamide, 1.0-5.0wt% cross-linking agent, 0-10.0wt% carboxyxylan, and 1.0-5.0wt% lignosulfonate into 20 mL deionized water. And stir at room temperature for 2h, then add 0.5-2.5wt% initiator and 0.5-2.5wt% tetramethylethylenediamine, stir evenly, and then further polymerize the resulting solution at room temperature for 12h to obtain water. gel; 2)用去离子水洗涤水凝胶,然后放入冷冻干燥机中,在-50℃下干燥48h后得二元复配木质素基气凝胶吸附材料。2) Wash the hydrogel with deionized water, then put it into a freeze dryer and dry it at -50°C for 48 hours to obtain a binary compound lignin-based airgel adsorption material. 7.权利要求1-5任意一项所述的一种二元复配木质素基气凝胶吸附材料用于吸附印染废水中的亚甲基蓝。7. A binary compound lignin-based airgel adsorption material according to any one of claims 1 to 5 is used to adsorb methylene blue in printing and dyeing wastewater. 8.根据权利要求7所述的应用,其特征在于,方法如下:调节亚甲基蓝溶液的pH值1-14,向其中加入二元复配木质素基气凝胶吸附材料进行吸附。8. The application according to claim 7, characterized in that the method is as follows: adjust the pH value of the methylene blue solution to 1-14, and add a binary compound lignin-based airgel adsorption material therein for adsorption. 9.根据权利要求8所述的应用,其特征在于,所述亚甲基蓝溶液的浓度为10-200mg/mL,体积为50mL;二元复配木质素基气凝胶吸附材料的用量为0.01-0.09g。9. The application according to claim 8, characterized in that the concentration of the methylene blue solution is 10-200 mg/mL and the volume is 50 mL; the dosage of the binary compound lignin-based airgel adsorption material is 0.01-0.09 g. 10.根据权利要求8所述的应用,其特征在于,所述吸附的条件为:吸附温度为10-80℃,吸附时间为5-1440min。10. The application according to claim 8, characterized in that the adsorption conditions are: adsorption temperature is 10-80°C, and adsorption time is 5-1440 min.
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