CN114160554B - Method for treating waste cation exchange resin containing radioactive elements by using ternary carbonic acid eutectic molten salt - Google Patents
Method for treating waste cation exchange resin containing radioactive elements by using ternary carbonic acid eutectic molten salt Download PDFInfo
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- 239000003729 cation exchange resin Substances 0.000 title claims abstract description 44
- 239000002699 waste material Substances 0.000 title claims abstract description 40
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 230000002285 radioactive effect Effects 0.000 title claims abstract description 28
- 230000005496 eutectics Effects 0.000 title claims abstract description 24
- 150000003839 salts Chemical class 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 16
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 title claims abstract description 12
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims abstract description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 13
- 239000011833 salt mixture Substances 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 9
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 7
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 7
- 229910000027 potassium carbonate Inorganic materials 0.000 claims abstract description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 7
- 229940023913 cation exchange resins Drugs 0.000 claims abstract description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- 229910017052 cobalt Inorganic materials 0.000 abstract description 15
- 239000010941 cobalt Substances 0.000 abstract description 15
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract description 15
- 239000011347 resin Substances 0.000 abstract description 15
- 229920005989 resin Polymers 0.000 abstract description 15
- 238000005341 cation exchange Methods 0.000 abstract description 5
- 230000000717 retained effect Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 4
- 238000005342 ion exchange Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000004568 cement Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000009616 inductively coupled plasma Methods 0.000 description 3
- 125000002091 cationic group Chemical group 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- CHRJZRDFSQHIFI-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;styrene Chemical group C=CC1=CC=CC=C1.C=CC1=CC=CC=C1C=C CHRJZRDFSQHIFI-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000001723 curing Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000012508 resin bead Substances 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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Abstract
一种用三元碳酸共晶熔盐处理含放射性元素的废弃阳离子交换树脂的方法。本发明属于废弃树脂处理领域。本发明为解决现有处理阳离子交换废树脂的方法存在的放射性核素被废气夹带排出、难以固定的技术问题。本发明的方法按以下步骤进行：步骤1：将碳酸锂、碳酸钠和碳酸钾混合均匀，得到三元共晶盐混合物，然后加入含放射性元素的废弃阳离子交换树脂继续混合均匀；步骤2：将步骤1后的混合物在750～850℃下加热处理1.5h～2.5h，完成含放射性元素的废弃阳离子交换树脂的处理。本发明通过三元碳酸共晶熔盐的用量及处理温度的综合调控，实现了在大幅度降低三元碳酸共晶熔盐用量的基础上高效处理含钴阳离子交换树脂的目的，大部分的钴仍被保留在熔盐中，处理效果显著。
A method for treating waste cation exchange resin containing radioactive elements with ternary carbonic acid eutectic molten salt. The invention belongs to the field of waste resin treatment. The invention aims to solve the technical problem that radioactive nuclides are entrained and discharged by exhaust gas and difficult to be fixed in the existing method for treating cation exchange waste resin. The method of the present invention is carried out according to the following steps: Step 1: Lithium carbonate, sodium carbonate and potassium carbonate are mixed homogeneously, obtain ternary eutectic salt mixture, then add the discarded cation exchange resin containing radioactive element and continue to mix homogeneously; Step 2: Mix The mixture after step 1 is heat-treated at 750-850°C for 1.5h-2.5h to complete the treatment of waste cation exchange resins containing radioactive elements. The present invention realizes the purpose of efficiently treating the cobalt-containing cation exchange resin on the basis of greatly reducing the dosage of the ternary carbonic acid eutectic molten salt through the comprehensive regulation and control of the dosage of the ternary carbonic acid eutectic molten salt, and most of the cobalt It is still retained in the molten salt, and the treatment effect is remarkable.
Description
技术领域technical field
本发明属于废弃树脂处理领域，具体涉及一种用三元碳酸共晶熔盐处理含放射性元素的废弃阳离子交换树脂的方法。The invention belongs to the field of waste resin treatment, and in particular relates to a method for treating waste cation exchange resin containing radioactive elements with ternary carbonic acid eutectic molten salt.
背景技术Background technique
阳离子树脂在核工业中被广泛用于去除放射性污染物。装载有放射性核素的树脂不能再生和利用，它们应得到合理的处理以最大限度地减少对环境的危害。Cationic resins are widely used in the nuclear industry to remove radioactive contaminants. Resins loaded with radionuclides cannot be regenerated and utilized, and they should be treated reasonably to minimize harm to the environment.
常见的处理废树脂的方法包括水泥固化、焚烧、热解等。由于水泥粘合剂和树脂珠粒之间缺乏适当的粘附力，用水泥固化方法处理树脂废料时，常存在着包容量低、固化体增容比较大、核素浸出率高等问题。传统热解或焚烧虽然能最大限度的减少废物体积，但是放射性核素会随着尾气的排放而逸散到空气中。因此在处理废树脂时，不仅要遵循废物最小化的原则，彻底地处理掉废树脂，同时也要有效地截留放射性核素、减少其逃逸。Common methods of processing waste resin include cement solidification, incineration, pyrolysis, etc. Due to the lack of proper adhesion between the cement binder and the resin beads, when the resin waste is treated by the cement curing method, there are often problems such as low containment capacity, large volume expansion ratio of the solidified body, and high nuclide leaching rate. Although traditional pyrolysis or incineration can minimize the volume of waste, radionuclides will dissipate into the air along with exhaust emissions. Therefore, when dealing with waste resins, not only should the principle of waste minimization be followed to completely dispose of waste resins, but also radionuclides should be effectively intercepted to reduce their escape.
发明内容Contents of the invention
本发明为解决现有处理阳离子交换废树脂的方法存在的放射性核素被废气夹带排出、难以固定的技术问题，而提供了一种用三元碳酸共晶熔盐处理含放射性元素的废弃阳离子交换树脂的方法。In order to solve the technical problem that radioactive nuclides are entrained and discharged by exhaust gas and difficult to fix in the existing method for treating cation exchange waste resin, the present invention provides a waste cation exchange method for treating waste cation exchange containing radioactive elements with ternary carbonic acid eutectic molten salt. Resin method.
本发明的一种用三元碳酸共晶熔盐处理含放射性元素的废弃阳离子交换树脂的方法按以下步骤进行：A kind of method of processing waste cation exchange resin containing radioactive element with ternary carbonic acid eutectic molten salt of the present invention is carried out as follows:
步骤1：将碳酸锂、碳酸钠和碳酸钾混合均匀，得到三元共晶盐混合物，然后加入含放射性元素的废弃阳离子交换树脂继续混合均匀；Step 1: Mix lithium carbonate, sodium carbonate and potassium carbonate uniformly to obtain a ternary eutectic salt mixture, then add waste cation exchange resin containing radioactive elements and continue to mix uniformly;
步骤2：将步骤1后的混合物在750～850℃下加热处理1.5h～2.5h，完成含放射性元素的废弃阳离子交换树脂的处理。Step 2: Heat the mixture after step 1 at 750-850°C for 1.5h-2.5h to complete the treatment of waste cation exchange resin containing radioactive elements.
进一步限定，步骤1中所述三元共晶盐混合物中碳酸锂、碳酸钠和碳酸钾的质量比为1：(0.78～1.16)：(0.89～1.33)。It is further defined that the mass ratio of lithium carbonate, sodium carbonate and potassium carbonate in the ternary eutectic salt mixture in step 1 is 1:(0.78-1.16):(0.89-1.33).
进一步限定，步骤1中所述三元共晶盐混合物中碳酸锂、碳酸钠和碳酸钾的质量比为1：0.97：1.11。It is further defined that the mass ratio of lithium carbonate, sodium carbonate and potassium carbonate in the ternary eutectic salt mixture in step 1 is 1:0.97:1.11.
进一步限定，步骤1中所述三元共晶盐混合物与含放射性元素的废弃阳离子交换树脂的质量比为(0.8～1.2)：1。It is further defined that the mass ratio of the ternary eutectic salt mixture to the waste cation exchange resin containing radioactive elements in step 1 is (0.8-1.2):1.
进一步限定，步骤1中所述三元共晶盐混合物与含放射性元素的废弃阳离子交换树脂的质量比为1：1。It is further defined that the mass ratio of the ternary eutectic salt mixture to the spent cation exchange resin containing radioactive elements in step 1 is 1:1.
进一步限定，步骤1中所述含放射性元素的废弃阳离子交换树脂为含Co的废弃阳离子交换树脂。It is further defined that the waste cation exchange resin containing radioactive elements in step 1 is waste cation exchange resin containing Co.
进一步限定，步骤1中所述含放射性元素的废弃阳离子交换树脂中放射性元素的含量为1.6wt％～2.4wt％。It is further defined that the content of radioactive elements in the waste cation exchange resin containing radioactive elements in step 1 is 1.6wt%-2.4wt%.
进一步限定，步骤1中所述含放射性元素的废弃阳离子交换树脂中放射性元素的含量为2wt％。It is further defined that the content of radioactive elements in the waste cation exchange resin containing radioactive elements in step 1 is 2wt%.
进一步限定，步骤2中将步骤1后的混合物在800℃下加热处理2h，完成含放射性元素的废弃阳离子交换树脂的处理。It is further defined that in
本发明与现有技术相比具有的显著效果：The remarkable effect that the present invention has compared with prior art:
本发明利用熔融碳酸盐中碳酸根可以与含钴阳离子交换树脂中钴反应，并将其氧化为四氧化三钴的特点，用三元碳酸共晶熔盐氧化含钴阳离子交换树脂，并将钴转变为了具有良好热稳定性的四氧化三钴，并通过三元碳酸共晶熔盐的用量及处理温度的综合调控，实现了在大幅度降低三元碳酸共晶熔盐的用量的基础上高效处理含钴阳离子交换树脂的目的，在800℃下氧化2h，氧化效率高达95.64％，钴的截留效率为97.3％，大部分的钴仍被保留在熔盐中。The present invention utilizes the characteristic that carbonate in molten carbonate can react with cobalt in cobalt-containing cation exchange resin, and oxidize it into tricobalt tetroxide, oxidize cobalt-containing cation exchange resin with ternary carbonic acid eutectic molten salt, and convert cobalt into Cobalt tetroxide with good thermal stability, and through the comprehensive control of the dosage of ternary carbonic acid eutectic molten salt and the comprehensive control of treatment temperature, it realizes efficient treatment of cobalt-containing cation exchange on the basis of greatly reducing the dosage of ternary carbonic acid eutectic molten salt The purpose of the resin is to oxidize at 800°C for 2 hours, the oxidation efficiency is as high as 95.64%, the cobalt interception efficiency is 97.3%, and most of the cobalt is still retained in the molten salt.
附图说明Description of drawings
图1为对比例1处理后的产物的XRD图；Fig. 1 is the XRD figure of the product after comparative example 1 processing;
图2为未进行离子交换的阳离子交换树脂的热重曲线图；Fig. 2 is the thermogravimetric curve diagram of the cation exchange resin that does not carry out ion exchange;
图3为实施例1处理后的产物的XRD图。Fig. 3 is the XRD pattern of the product treated in Example 1.
具体实施方式Detailed ways
实施例1、本实施例的一种用三元碳酸共晶熔盐处理含放射性元素的废弃阳离子交换树脂的方法按以下步骤进行：Embodiment 1, a kind of method of processing waste cation exchange resin containing radioactive elements with ternary carbonic acid eutectic molten salt of the present embodiment is carried out as follows:
步骤1：将碳酸锂、碳酸钠和碳酸钾按照质量比1：0.97：1.11混合均匀，得到三元共晶盐混合物，然后加入含Co的废弃阳离子交换树脂继续混合均匀；所述三元共晶盐混合物与含Co的废弃阳离子交换树脂的质量比为1：1；所述含Co的废弃阳离子交换树脂中Co的含量为2wt％；Step 1: Mix lithium carbonate, sodium carbonate and potassium carbonate uniformly according to the mass ratio of 1:0.97:1.11 to obtain a ternary eutectic salt mixture, then add waste cation exchange resin containing Co and continue to mix uniformly; the ternary eutectic The mass ratio of the salt mixture to the waste cation exchange resin containing Co is 1:1; the content of Co in the waste cation exchange resin containing Co is 2wt%;
步骤2：将步骤1后的混合物在800℃下加热处理2h，完成Co的废弃阳离子交换树脂的处理。Step 2: Heat the mixture after step 1 at 800° C. for 2 h to complete the treatment of Co waste cation exchange resin.
本实施例中Co含量为2wt％的废弃阳离子交换树脂按下述步骤模拟获得：In this embodiment, the waste cation exchange resin with a Co content of 2wt% is simulated according to the following steps:
步骤(1)：称量0.4g无水CoCl2，充分溶解后定容至50mL，制备成浓度为0.0615mol/L的CoCl2水溶液来模拟含有放射性核素的废水；Step (1): Weigh 0.4g of anhydrous CoCl 2 , fully dissolve it and set the volume to 50mL, and prepare a CoCl 2 aqueous solution with a concentration of 0.0615mol/L to simulate wastewater containing radionuclides;
步骤(2)：①使用1mol/LHCl溶液充分浸润阳离子交换树脂(杭州争光树脂厂生产的核级732型阳离子交换树脂，其结构为苯环上带有磺酸基官能团的苯乙烯-二乙烯苯共聚物)2h，然后使用去离子水冲洗阳离子树脂7-8次至溶液pH值为7；②使用1mol/LNaOH溶液充分浸润阳离子交换树脂2h，然后使用去离子水冲洗阳离子树脂7-8次至溶液pH值为7；重复步骤①-②的操作3-5次，然后将阳离子交换树脂在湿态下保存，得到预处理后阳离子交换树脂；Step (2): ① use 1mol/L HCl solution to fully infiltrate the cation exchange resin (nuclear grade 732 type cation exchange resin produced by Hangzhou Zhengguang Resin Factory, its structure is styrene-divinylbenzene with sulfonic acid functional group on the benzene ring copolymer) for 2 hours, then rinse the cationic resin with deionized water for 7-8 times until the pH value of the solution is 7; The pH value of the solution is 7; repeat steps ①-② for 3-5 times, and then store the cation exchange resin in a wet state to obtain the pretreated cation exchange resin;
步骤(3)：取5mL步骤1得到的溶液与2g步骤2得到的预处理后的阳离子交换树脂置于10mL离心管中，在25℃温度下，以120r/min的转速震荡48h，完成离子交换，然后将离子交换后的树脂在101℃条件下干燥12h，获得Co含量为2wt％的废弃阳离子交换树脂。Step (3): Take 5mL of the solution obtained in step 1 and 2g of the pretreated cation exchange resin obtained in
对比例1：本实施例与实施例1不同的是：待处理树脂为未进行离子交换的阳离子交换树脂(杭州争光树脂厂生产的核级732型阳离子交换树脂，其结构为苯环上带有磺酸基官能团的苯乙烯-二乙烯苯共聚物)。Comparative Example 1: The difference between this embodiment and Example 1 is that the resin to be treated is a cation-exchange resin without ion exchange (the nuclear grade 732 type cation-exchange resin produced by Hangzhou Zhengguang Resin Factory has a structure of benzene ring with Styrene-divinylbenzene copolymers with sulfonic acid functional groups).
对比例1处理后的产物的XRD图如图1所示，从图1可以看出，在800℃下氧化阳离子交换树脂2h，废盐中包括NaK3(SO4)2，这表明产生的SO2被碳酸熔盐有效地吸收并转变成了稳定的无机物。The XRD pattern of the product treated in Comparative Example 1 is shown in Figure 1. It can be seen from Figure 1 that the cation exchange resin was oxidized at 800°C for 2 hours, and the waste salt included NaK 3 (SO 4 ) 2 , which indicated that the produced SO 2 is effectively absorbed by the carbonate molten salt and transformed into a stable inorganic substance.
未进行离子交换的阳离子交换树脂的热重曲线如图2所示，从图2可以看出，在800℃下氧化2h，阳离子交换树脂就能被有效地破坏。The thermogravimetric curve of the cation exchange resin without ion exchange is shown in Figure 2. It can be seen from Figure 2 that the cation exchange resin can be effectively destroyed by oxidation at 800°C for 2 hours.
本发明实施例1处理后的产物的XRD图如图3所示，从图3可以看出，钴四氧化三钴的形式存在。综上可以看出三元碳酸共晶盐熔盐法是一种有效处理含钴阳离子交换树脂、截留放射性核素钴的方法。The XRD pattern of the processed product in Example 1 of the present invention is shown in FIG. 3 , and it can be seen from FIG. 3 that cobalt exists in the form of tricobalt tetroxide. In summary, it can be seen that the ternary carbonate eutectic salt molten salt method is an effective method for treating cobalt-containing cation exchange resins and intercepting radionuclide cobalt.
利用电感耦合等离子技术ICP，采用德国赛默飞世尔的电感耦合等离子发射仪对实施例1处理后的产物中的Co2+含量进行检测，检测参数如下：功率为1150W，冲洗20s，长波10s，短波5s，每个样品重复测量3次。结果显示，在800℃下氧化2h，氧化效率高达95.64％，钴的截留效率为97.3％，大部分的钴仍被保留在熔盐中。Utilize the inductively coupled plasma technology ICP, adopt the inductively coupled plasma launcher of German Thermo Fisher to detect the Co content in the product after the treatment of embodiment 1, and the detection parameters are as follows: power is 1150W, flushing 20s, long wave 10s , short-wave 5s, repeat the measurement 3 times for each sample. The results show that after oxidation at 800°C for 2 hours, the oxidation efficiency is as high as 95.64%, the cobalt interception efficiency is 97.3%, and most of the cobalt is still retained in the molten salt.
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