技术领域technical field
本发明属于对铀吸附的技术领域，涉及一种以大孔聚N-异丙基丙烯酰胺/壳聚糖（简称大孔PNIPAAm/CS，下同）半互穿网络温敏水凝胶来吸附铀的方法。The invention belongs to the technical field of uranium adsorption, and relates to a method for adsorbing uranium with a semi-interpenetrating network temperature-sensitive hydrogel of macroporous poly N-isopropylacrylamide/chitosan (abbreviated as macroporous PNIPAAm/CS, the same below). method.
背景技术Background technique
铀（uranium，简称U），是一种十分重要的能源物资，在工业、农业、国防和科学技术中都具有重要意义。铀作为一种核燃料，在核反应堆中可释放巨大的能量。轻水反应堆中，1吨的天然铀相当于15～17千吨煤，用于发电可达45～50兆度；快中子增殖堆中，1吨天然铀相当于100万吨煤左右，可发电约30亿度。同时核燃料还广泛用于交通运输工具中推进动力方面。核燃料产生的核动力堆可用于潜艇、远洋货轮，核燃料负荷量和续航能力，是一般燃料无法比拟的。铀也可以作为核炸药，能用作核武器的装料。铀核裂变时可以产生300多种核素，这些核素及其产生射线在各方面的应用为核能的和平利用开辟了另一个广阔的领域。同时，铀也可作为热核武器氢弹的引爆剂，铀核裂变时产生的200多种放射性同位素，经分离后广泛用于国民经济各个部门，如农业上用于辐照育种，食品工业用于食品保鲜灭菌，医药上用于放射治疗，工业上用于无损探伤、地质勘探、文物考古等。铀资源的充分利用是国家经济健康、平稳发展的战略需求。因而，在开展采铀方面的新技术研究，提高矿产资源利用率的同时，必须注重从铀采冶产生的放射性废水中提取铀，以提高铀的综合利用率。同时，铀矿开采过程中产生的废水污染不仅会影响周边地区的水质，而且对矿区周围植物、农田和土壤产生不可逆转的污染，影响生物的生存和公众的健康。Uranium (U) is a very important energy material, which is of great significance in industry, agriculture, national defense and science and technology. As a nuclear fuel, uranium can release huge amounts of energy in nuclear reactors. In a light water reactor, 1 ton of natural uranium is equivalent to 15-17 thousand tons of coal, which can reach 45-50 megawatts for power generation; in a fast neutron breeder reactor, 1 ton of natural uranium is equivalent to about 1 million tons of coal, which can Power generation is about 3 billion kWh. At the same time, nuclear fuel is also widely used in propulsion power in transportation vehicles. The nuclear power reactor produced by nuclear fuel can be used in submarines and ocean-going cargo ships. The nuclear fuel load and endurance are unmatched by general fuel. Uranium can also be used as a nuclear explosive and can be used as a fuel for nuclear weapons. The nuclear fission of uranium can produce more than 300 kinds of nuclides, and the application of these nuclides and the rays produced in various aspects has opened up another broad field for the peaceful use of nuclear energy. At the same time, uranium can also be used as a detonator for thermonuclear hydrogen bombs. More than 200 radioactive isotopes produced during uranium nuclear fission are widely used in various sectors of the national economy after separation, such as radiation breeding in agriculture and food in the food industry. Fresh-keeping and sterilization, used in medicine for radiation therapy, industrially used for non-destructive flaw detection, geological exploration, cultural relics and archaeology, etc. The full utilization of uranium resources is a strategic requirement for the healthy and stable development of the national economy. Therefore, while carrying out new technology research on uranium mining and improving the utilization rate of mineral resources, attention must be paid to extracting uranium from radioactive wastewater produced by uranium mining and smelting to improve the comprehensive utilization rate of uranium. At the same time, the wastewater pollution generated during uranium mining will not only affect the water quality in surrounding areas, but also cause irreversible pollution to plants, farmland and soil around the mining area, affecting the survival of organisms and public health.
目前常用的分离、富集铀的方法有化学沉淀、离子交换、溶剂萃取、过滤和反向渗透等，但这些方法存在着产生新化学污染、能耗高、操作烦琐和成本高昂等缺点，限制了它们的应用。与这些方法相比，吸附法具有吸附材料来源广泛、成本低廉、选择性高、速率快和容量大等优点。吸附法是一种对溶解态污染物的物理化学分离技术，主要是让废水与具有吸附性能的固体吸附剂接触，从而使废水中的有毒有害的物质附着在吸附剂表面上，进而将废水中有毒有害物质除去。吸附法的关键是吸附剂的吸附性能，常见用于吸附去除水溶液中铀的吸附剂主要有有机聚合物、粘土类、生物质类及岩石等。但一般都存在着吸附能力强但脱附较困难、机械强度较差、吸附和脱附过程较难控制等不足，因此，开发出一种新型吸附剂，使其具有较大的吸附表面积、机械强度好、吸附和脱附过程可控、对铀吸附量高，不仅具有重要的理论意义，而且具有实际应用价值。At present, the commonly used methods for separating and enriching uranium include chemical precipitation, ion exchange, solvent extraction, filtration and reverse osmosis, etc., but these methods have disadvantages such as new chemical pollution, high energy consumption, cumbersome operation and high cost. their application. Compared with these methods, the adsorption method has the advantages of wide source of adsorption materials, low cost, high selectivity, fast rate and large capacity. Adsorption method is a physical and chemical separation technology for dissolved pollutants. It mainly makes wastewater contact with a solid adsorbent with adsorption properties, so that toxic and harmful substances in wastewater are attached to the surface of the adsorbent, and then the waste water Toxic and harmful substances are removed. The key to the adsorption method is the adsorption performance of the adsorbent. Commonly used adsorbents for adsorption and removal of uranium in aqueous solution mainly include organic polymers, clays, biomass and rocks. However, there are generally deficiencies such as strong adsorption capacity but difficult desorption, poor mechanical strength, and difficult control of the adsorption and desorption process. Therefore, a new type of adsorbent has been developed to have a large adsorption surface area and mechanical It has good strength, controllable adsorption and desorption process, and high adsorption capacity for uranium, which not only has important theoretical significance, but also has practical application value.
发明内容Contents of the invention
本发明的目的是提供一种吸附铀的方法，即一种以大孔PNIPAAm/CS半互穿网络温敏水凝胶吸附铀的方法，所述方法制备出的吸附剂具有较大的吸附表面积、机械强度较好、吸附和脱附过程可控、且对铀具有高的吸附量。The purpose of the present invention is to provide a method for adsorbing uranium, that is, a method for adsorbing uranium with a macroporous PNIPAAm/CS semi-interpenetrating network thermosensitive hydrogel, the adsorbent prepared by the method has a large adsorption surface area, mechanical It has good strength, controllable adsorption and desorption process, and high adsorption capacity for uranium.
本发明吸附铀的方法如下：首先利用乳液聚合的方法，以司班-80为乳化剂，N,N′-亚甲基双丙烯酰胺（MBA）为交联剂，过硫酸铵（APS）为引发剂，N,N,N′,N′-四甲基乙二胺（TEMED）为促进剂，制备出大孔PNIPAAm/CS半互穿网络温敏型铀吸附剂。然后将制得的大孔PNIPAAm/CS半互穿网络凝胶经冷冻干燥后加入到锥形瓶中，再加入一定浓度的铀溶液，用NaOH溶液或HNO3溶液调节铀溶液的pH值，在振荡器上以200 r/min振荡至吸附平衡。取出待测样液，在待测样中加入 pH=2.5的氯乙酸-乙酸钠缓冲液和偶氮胂Ⅲ并定容，根据吸附平衡公式即可计算出吸附容量（qe）。The method for adsorbing uranium in the present invention is as follows: firstly, the method of emulsion polymerization is used, with Span-80 as emulsifier, N,N′-methylenebisacrylamide (MBA) as crosslinking agent, and ammonium persulfate (APS) as The macroporous PNIPAAm/CS semi-interpenetrating network temperature-sensitive uranium adsorbent was prepared with N,N,N′,N′-tetramethylethylenediamine (TEMED) as the initiator. Then put the prepared macroporous PNIPAAm/CS semi-IPN gel into the Erlenmeyer flask after freeze-drying, then add a certain concentration of uranium solution, adjust the pH value of the uranium solution with NaOH solution or HNO3 solution, and shake Oscillating at 200 r/min to adsorption equilibrium. Take out the sample solution to be tested, add chloroacetic acid-sodium acetate buffer solution with pH=2.5 and arsine azo III to the sample to be tested and constant volume, then calculate the adsorption capacity (qe) according to the adsorption equilibrium formula.
本发明的吸附剂制备步骤如下：The preparation steps of adsorbent of the present invention are as follows:
1）称取0.5-1.0g壳聚糖单体溶于乙酸中，加入N-异丙基丙烯酰胺（NIPAAm）单体和N,N′-亚甲基双丙烯酰胺（MBA）交联剂，混合均匀。1) Weigh 0.5-1.0g chitosan monomer and dissolve it in acetic acid, add N-isopropylacrylamide (NIPAAm) monomer and N,N′-methylenebisacrylamide (MBA) cross-linking agent, well mixed.
2）在搅拌状态下加入聚乙烯醇（PVA）稳定剂，乳化剂Span-80，搅拌5-10 min后加入过硫酸铵（APS）引发剂和N,N,N′,N′-四甲基乙二胺（TEMED）促进剂。2) Add polyvinyl alcohol (PVA) stabilizer and emulsifier Span-80 while stirring, add ammonium persulfate (APS) initiator and N,N,N′,N′-tetramethyl after stirring for 5-10 minutes ethylenediamine (TEMED) accelerator.
3）搅拌10-15 min后静置24 h后，取出凝胶，用乙醇洗去Span-80和PVA制孔剂，再用蒸馏水浸泡45-48 h，定时换水以除去未反应单体、残余引发剂或催化剂，最后将凝胶切成块，冷冻干燥备用。在聚乙烯醇（PVA），Span-80，过硫酸铵（APS）、N,N,N′,N′-四甲基乙二胺（TEMED）全部混合搅拌后，静置时间为20-30h。3) After stirring for 10-15 minutes and standing for 24 hours, take out the gel, wash off Span-80 and PVA pore-forming agent with ethanol, then soak in distilled water for 45-48 hours, and change the water regularly to remove unreacted monomers, The residual initiator or catalyst is finally cut into pieces and freeze-dried for later use. After polyvinyl alcohol (PVA), Span-80, ammonium persulfate (APS), N,N,N',N'-tetramethylethylenediamine (TEMED) are all mixed and stirred, the standing time is 20-30h .
吸附剂的制备方法中，乙酸溶液的质量分数为5%-10%。In the preparation method of the adsorbent, the mass fraction of the acetic acid solution is 5%-10%.
吸附剂的制备方法中，壳聚糖单体、N-异丙基丙烯酰胺（NIPAAm）单体、N,N′-亚甲基双丙烯酰胺（MBA）的质量比为1:20-50:1。In the preparation method of the adsorbent, the mass ratio of chitosan monomer, N-isopropylacrylamide (NIPAAm) monomer, and N,N′-methylenebisacrylamide (MBA) is 1:20-50: 1.
吸附剂的制备方法中，聚乙烯醇（PVA）稳定剂加入量为0.5-0.8mL。In the preparation method of the adsorbent, the addition amount of the polyvinyl alcohol (PVA) stabilizer is 0.5-0.8mL.
吸附剂的制备方法中，Span-80乳化剂加入量为0.5-1.0mL。In the preparation method of the adsorbent, the amount of Span-80 emulsifier added is 0.5-1.0mL.
吸附剂的制备方法中，过硫酸铵（APS）引发剂加入量为0.01-0.05g。In the preparation method of the adsorbent, the addition amount of the ammonium persulfate (APS) initiator is 0.01-0.05g.
吸附剂的制备方法中，TEMED促进剂加入量为50-100μL。In the preparation method of the adsorbent, the amount of the TEMED accelerator added is 50-100 μL.
附图说明Description of drawings
图1为大孔凝胶的扫描电镜放大倍数为5000倍图，Figure 1 is a scanning electron microscope magnification of 5000 times for the macroporous gel,
图2为大孔凝胶的扫描电镜放大倍数为25000倍图，Figure 2 is a scanning electron microscope magnification of 25,000 times for the macroporous gel,
图3为大孔凝胶未吸附过铀的红外光谱图，Fig. 3 is the infrared spectrogram of macroporous gel without adsorbing uranium,
图4吸附时间对大孔PNIPAAm/CS半互穿网络水凝胶吸附铀的影响变化曲线，Figure 4 The curve of the effect of adsorption time on the adsorption of uranium by macroporous PNIPAAm/CS semi-IPN hydrogel,
图5大孔PNIPAAm/CS半互穿网络水凝胶对铀的变温吸附曲线。Fig. 5 Temperature swing adsorption curve of macroporous PNIPAAm/CS semi-IPN hydrogel for uranium.
具体实施方式Detailed ways
以下实施例是本发明的进一步说明，而不是限制本发明的范围。The following examples are further illustrations of the present invention, rather than limiting the scope of the present invention.
实施例1Example 1
1）准确称取0.5g壳聚糖单体溶于质量分数为5 %的乙酸中，加入15 gNIPAAm单体和0.5g交联剂MBA，混合均匀。1) Accurately weigh 0.5g of chitosan monomer and dissolve it in acetic acid with a mass fraction of 5%, add 15g of NIPAAm monomer and 0.5g of cross-linking agent MBA, and mix well.
2）在搅拌状态下加入0.6 mL乳化剂稳定剂PVA，0.8 mL乳化剂Span-80，搅拌5-10 min后加入0.03 g引发剂APS和60 μL促进剂TEMED。2) Add 0.6 mL of emulsifier stabilizer PVA and 0.8 mL of emulsifier Span-80 under stirring. After stirring for 5-10 min, add 0.03 g of initiator APS and 60 μL of accelerator TEMED.
3）搅拌10-15 min后静置24 h后，取出凝胶，用乙醇洗去制孔剂Span-80和PVA，再用蒸馏水浸泡48 h，定时换水以除去未反应单体，残余引发剂或催化剂，最后将凝胶切成块，冷冻干燥备用。3) After stirring for 10-15 min and standing for 24 h, take out the gel, wash off the pore-forming agent Span-80 and PVA with ethanol, then soak in distilled water for 48 h, change the water regularly to remove unreacted monomers, and residual triggers agent or catalyst, and finally the gel was cut into pieces and freeze-dried for later use.
图1为大孔凝胶的扫描电镜图，放大倍数为5000倍，图2放大倍数为25000倍。从图中可以看到，凝胶内部有明显的孔洞结构，孔洞的直径约在3 μm左右。结果表明，制备的相互连通的孔结构，增加了凝胶同铀溶液的接触面积，有利于大孔PNIPAAm/CS半互穿网络凝胶对铀的吸附。Figure 1 is the scanning electron microscope image of the macroporous gel with a magnification of 5,000 times, and Figure 2 is a magnification of 25,000 times. It can be seen from the figure that there is an obvious pore structure inside the gel, and the diameter of the pore is about 3 μm. The results show that the interconnected pore structure increases the contact area between the gel and the uranium solution, which is beneficial to the adsorption of uranium by the macroporous PNIPAAm/CS semi-interpenetrating network gel.
实施例2Example 2
利用实施例1制备的水凝胶考察对铀的吸附性能，准确称取三份0.03g凝胶，第一份作为对照样。第二份加入到70μg/mL的铀标准溶液中，在308.15K温度点振荡适当时间，每隔一定时间取1 mL上清液，加入2 mL缓冲溶液，2 mL偶氮胂Ⅲ，定容至25 mL，测定吸光度，分析吸附前后溶液中铀的浓度，计算铀的吸附量。第三份加入到70μg/mL的铀标准溶液中，在293.15K、323.15K两温度点振荡适当时间，每隔一定时间取1 mL上清液，加入2 mL缓冲溶液，2 mL偶氮胂Ⅲ，定容至25 mL，测定吸光度，计算铀的吸附量。The hydrogel prepared in Example 1 was used to investigate the adsorption performance of uranium, and three 0.03g gels were accurately weighed, and the first one was used as a control sample. Add the second part to 70μg/mL uranium standard solution, shake at 308.15K for an appropriate time, take 1 mL of supernatant at regular intervals, add 2 mL of buffer solution, 2 mL of arsine III, and dilute to 25 mL, measure the absorbance, analyze the concentration of uranium in the solution before and after adsorption, and calculate the amount of uranium adsorbed. Add the third part to 70μg/mL uranium standard solution, shake at two temperature points of 293.15K and 323.15K for an appropriate time, take 1 mL of supernatant at regular intervals, add 2 mL of buffer solution, 2 mL of arsenazo III , set the volume to 25 mL, measure the absorbance, and calculate the adsorption amount of uranium.
图3为大孔凝胶未吸附过铀的红外光谱图，从图3可以看出，在3400 cm-1左右处出现了壳聚糖的O-H和-NH2的伸缩振动峰，而在2972 cm-1和2852 cm-1处分别属于壳聚糖内的-CH2的对称和非对称吸收峰，在1386 cm-1处观察到C-N键的较强的吸收峰。图4是凝胶吸附铀后的红外图谱。吸附铀后在910 cm-1附近有一个很明显的吸收峰，这是铀酰离子的特征峰。在1550 cm-1处也出现了一个吸收峰，这是仲胺(-N-H)的特征峰，在1625 cm-1处出现吸收峰，这是酰胺(-CO-NH-)的特征峰，说明凝胶表面的氨基已经转变为酰胺，也即与铀酰离子螯合，表明该凝胶成功地吸附了水体中的铀酰离子。Figure 3 is the infrared spectrogram of the macroporous gel that has not adsorbed uranium. It can be seen from Figure 3 that the stretching vibration peaks of O-H and -NH2 of chitosan appeared at about 3400 cm-1, while at 2972 cm-1 The 1 and 2852 cm-1 belong to the symmetric and asymmetric absorption peaks of -CH2 in chitosan, respectively, and the stronger absorption peak of the C-N bond is observed at 1386 cm-1. Figure 4 is the infrared spectrum of the gel adsorbed uranium. After uranium is adsorbed, there is an obvious absorption peak around 910 cm-1, which is a characteristic peak of uranyl ions. There is also an absorption peak at 1550 cm-1, which is the characteristic peak of secondary amine (-N-H), and an absorption peak appears at 1625 cm-1, which is the characteristic peak of amide (-CO-NH-), indicating The amino groups on the surface of the gel have been transformed into amides, that is, chelated with uranyl ions, indicating that the gel has successfully adsorbed uranyl ions in water.
图4吸附时间对大孔PNIPAAm/CS半互穿网络水凝胶吸附铀的影响变化曲线，从图中可以看出，凝胶在2 h左右达到吸附平衡，吸附容量为112 mg/g，说明对铀的吸附量高。Figure 4. The curve of the effect of adsorption time on the adsorption of uranium by the macroporous PNIPAAm/CS semi-IPN hydrogel. It can be seen from the figure that the gel reached adsorption equilibrium in about 2 h, and the adsorption capacity was 112 mg/g, indicating that High adsorption capacity for uranium.
图5大孔PNIPAAm/CS半互穿网络水凝胶对铀的变温吸附曲线。Fig. 5 Temperature swing adsorption curve of macroporous PNIPAAm/CS semi-IPN hydrogel for uranium.
当温度反复改变时，对铀的吸附量也通过温度的变化而改变。实验结果表明，通过简单的改变温度条件，可以很好的控制大孔凝胶的吸附与解吸，达到了实验的最终的目的。When the temperature is changed repeatedly, the adsorption amount of uranium is also changed by the temperature change. The experimental results show that by simply changing the temperature conditions, the adsorption and desorption of the macroporous gel can be well controlled, and the ultimate goal of the experiment is achieved.
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| WD01 | Invention patent application deemed withdrawn after publication | Application publication date:20150527 |