磷酸镁水泥固化中低放射性废物研究
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摘要
水泥固化技术运用在中低放射性废物的处理有着明显的优势，固化处理工艺和设备简单，处理费用低廉，固化体安全耐久，因此在中低放射性废物的固化和储存运输方面，均得到广泛应用。采用普通硅酸盐水泥和高铝水泥等的传统水泥处理技术存在水灰比高、核素浸出率高和固化体强度低等不足，而且放射性废物的pH值必须在一定范围，否则需进行预处理，同时放射性废物中PO43-, BO33-, Zn,Sn等离子影响水泥凝结时间和强度发展，特别是传统水泥固化体包容量小，固化体的储存或运输材料体积过大，一些情况下对于中低放射性废物的固化受到空间限制。因此，有必要从胶凝材料体系上选择新的水泥类型用于中低放射性废物固化，改善水泥固化体性能、提高固化体包容量，以及提高水泥固化速度和固化体安全耐久，促进水泥固化技术在核废料处理和处置领域应用。考虑磷酸镁水泥所具有的特点，本文研究选用磷酸镁水泥作为固化基材，将磷酸镁水泥用于固化中低放射性废物，包括用于处理中低放射性焚烧灰。
首先，从有利于中低放射性废物固化角度，研究磷酸镁水泥有关性能。对常用的三种磷酸盐分别制备的磷酸镁水泥强度以及配比对强度的影响进行研究，以便从中选择适宜的固化基材配方。同时考虑到磷酸镁水泥固化体在制备、储存和运输过程中可能受到温度变化的影响，研究了磷酸镁水泥在-20℃条件下养护强度发展趋势以及在经历高温后性能的变化情况。材料的耐久性也是重要的指标，因此对磷酸镁水泥的抗冻融性能和抗浸泡性能进行研究。结果显示采用磷酸二氢铵制备的磷酸镁水泥强度最大，磷酸二氢钾次之，磷酸氢二铵强度最低。配比对性能的影响，M/P比在其中起到关键作用，其次是硼砂的影响，氧化镁细度影响最小。磷酸镁水泥在低温条件下强度仍能实现较大的增长，而经历高温后，强度有所降低，但经历了1400℃处理后仍能保持结构的完整。而耐久性的研究也表明磷酸镁水泥具有较好的抗冻融循环和抗浸泡性能。通过对强度、温度对基材性能的影响以及耐久性的研究分析，表明磷酸镁水泥是一种理想的固化基材。
由于Cs和Sr是中低放射性废物中最常见且危害最大的两种放射性核素，通过掺加Cs和Sr研究了Cs和Sr对磷酸镁水泥水化和硬化的影响，磷酸镁水泥对Cs和Sr的吸附性能、含核素固化体的浸出率以及耐久性、以及Cs和Sr在磷酸镁水泥中的存在状态。掺加Cs和Sr均对磷酸镁水泥的抗压强度造成影响，造成了磷酸镁水泥强度的下降。磷酸镁水泥对Cs和Sr均具有较好的吸附性能，尤其对Sr吸附率高达97.72%。掺加Cs的固化体42d浸出率和累计浸出分数低至5.47×10-5cm·d-1和2.81×10-3cm，而掺加Sr的固化体Sr的42d浸出率和累计浸出分数可达2.85×10~(-5)cm·d~(-1)和5.92×10~(-3)cm。Cs对磷酸镁水泥早期水化影响较小，而Sr的影响较大，Sr的掺入降低了磷酸镁水泥的水化热，延缓了水化。Cs和Sr在固化体中主要以难溶的MgCsPO4·6H_2O和SrHPO_4形式存在，使其固化体浸出率大幅降低。
放射性焚烧灰是目前固化处理的难点。本文采用磷酸镁水泥固化模拟放射性焚烧灰。首先进行包容量研究，其次是对固化体的性能进行分析。通过强度分析，磷酸镁水泥对模拟焚烧灰的最大包容量可以达到60wt%。水化热分析表明模拟放射性焚烧灰掺量越大，固化体的水化热越低，导致水化进程有较大延缓。固化体Cs的浸出率为1.7×10-4cm·d~(-1)，累计浸出分数为0.15cm；Sr的浸出率为1.1×10-4cm·d~(-1)，累计浸出分数为0.015cm。对固化体的流动度，抗冲击性能、抗冻融性能和抗浸泡性能研究也表明了其完全满足固化体性能指标要求。
本研究表明，磷酸镁水泥对于中低放射性废物具有良好的固化性能。主要原因是由于核素与其它反应物形成了难溶的磷酸盐矿物，同时辅以磷酸镁水泥水化物的包裹作用，可快速将核素固定在固化体中，具有较大的废物包容量。因此磷酸镁水泥是一种理想的中低放射性废物固化基材。
Cement solidification process has significant advantage when applied in thedisposal of medium and low level radioactive wastes. Compared with othersolidification process, technology and equipment for cement solidification process isvery simple and low cost, solidified form also has good durability. So, cementsolidification process has been widely applied in storage and transportation of mediumand low level radioactive wastes. Traditional cement solidification technology hasmany disadvantages, such as high water to cement ratio, high nuclei leaching rate, lowsolidified form strength and etc. Traditional cement must cure under high pH valueenvironment，wastes need treatment previously. The setting time and strength ofcement may affected by PO43-, BO33-, Zn, Sn. Due to the disadvantages above,traditional cement solidification process has low wastes loading, which means morespace must remain to the storage, and the transportation of wastes is also a big problem.Therefore, the selection of new type cement for medium and low level radioactivewastes is necessary，the target of selection is improve the performance of the solidifiedform, improve the loading capacity and speed the solidification process, and finally getsolidified form with better durability, promote cement solidification process in the fieldof treatment and disposal of nuclear waste. Considering the characteristics ofmagnesium phosphate cement (MPC), magnesium phosphate cement was selected asmatrix material in this study for solidifying medium and low level radioactive waste,and solification of medium and low level radioactive incineration ash was also studied.
First of all, the related performances of magnesium phosphate cement which infavor of medium and low level radioactive wastes solidification were studied. In orderto select suitable matrix material, three kinds of phosphate were chose to preparationmagnesium phosphate cement; the effects of mix ration to the strength were alsostudied. Considering the preparation of solidified form of magnesium phosphatecement may be affected by the very low temperature, the strength development ofMPC was studied by curing under-20℃.The properties of MPC after various hightemperature treatments were also studied. Durability is also an important factor ofsolidified form, freezing and thawing test and soaking test were used to investigate thedurability of samples. Results show MPC prepared by ammonium dihydrogenphosphate has highest strength, the latter is MPC prepared by potassium dihydrogen phosphate, diammonium hydrogen phosphate is the worst. M/P plays a key role to thestrength of MPC, followed by effects of borax, particle size of magnesium oxide hasminimal effection. Strength of magnesium phosphate cement has been able to achievegrowth under low temperature conditions. Magnesium phosphate cement-basedmaterials have superior high-temperature performance, the structure of cement stillmaintain integrity even at up to1400℃, volume of samples will reduce under differenttemperature treatment, structural collapse did not occur whthin the full temperaturerange. Durability studies show that magnesium phosphate cement has good resistanceto freeze-thaw and soaking test. The results indicate magnesium phosphate cement isan ideal matrix material.
Secondly, because Cs and Sr are two of the most common and dangerest nuclei ofmedium and low level radioactive wastes, the solidification performance of MPC byadding Cs and Sr was studied. The affections of Sr and Cs addition to the strength ofMPC were studied, as well the hydration of MPC. The adsorption performance ofmagnesium phosphate cement to Cs, Sr was also studied. The durability and theexistence state of Cs and Sr in MPC were also investigated. Adding Cs and Sr causethe decline in the strength of MPC. Magnesium phosphate cement have betterperformance on adsorption Sr, absorption rate for Sr is up to97.72%. The42d leachingrates and cumulative leaching factor of solidified form with Cs are5.47x10-5cm·d-1and2.81x10-3cm respectively, and those of Sr are2.85x10-5cm·d-1and5.92x10-3cmrespectively. Sr addition reduces the hydration heat of hydration of magnesiumphosphate cement, slow hydration process, but those of Cs is not so significant.Cs andSr are mainly as MgCsPO4·6H2O and SrHPO4existed in the solidified form, so theleaching rates are significantly lower than other cement system,especially at the earlyleaching test.
Immobilization of radioactive incineration ash is a difficult in wastes diaposal.Magnesium phosphate cement was chosed to immbilizaton for simulated radioactiveincineration ash. The loading capacity of solidified form was studied, and theperformance of solidified form was also investigated. Through analysis of compressivestrength, maximum loading capacity of solidified form can reach60wt%. Hydrationheat analysis indicates with higher simulated radioactive incineration ash, the lowerhydration heat of solidified form can be found, caused the hydration process delay. Theleaching rate and cumulative leaching rate of solidified form can reach1.7×10-4cm·d-1and0.15cm for Cs,1.1×10-4cm·d~(-1)and0.015cm for Sr. fluidity of pastes, impact resistance, freezing and thawing resistance and anti soaking are fully met performancerequirements of solidified form.
This study showed that magnesium phosphate cement has good performance forsolidification of medium and low level radioactive waste. With the formation ofinsoluble phosphate mineral, and encapsulating with the hydration products of MPC,radioactive ions can be quickly fixed in the solidified form, and the final form has gooddurability. MPC is an ideal matrix material for medium and lowlevel radioactivewastes solidification.
首先，从有利于中低放射性废物固化角度，研究磷酸镁水泥有关性能。对常用的三种磷酸盐分别制备的磷酸镁水泥强度以及配比对强度的影响进行研究，以便从中选择适宜的固化基材配方。同时考虑到磷酸镁水泥固化体在制备、储存和运输过程中可能受到温度变化的影响，研究了磷酸镁水泥在-20℃条件下养护强度发展趋势以及在经历高温后性能的变化情况。材料的耐久性也是重要的指标，因此对磷酸镁水泥的抗冻融性能和抗浸泡性能进行研究。结果显示采用磷酸二氢铵制备的磷酸镁水泥强度最大，磷酸二氢钾次之，磷酸氢二铵强度最低。配比对性能的影响，M/P比在其中起到关键作用，其次是硼砂的影响，氧化镁细度影响最小。磷酸镁水泥在低温条件下强度仍能实现较大的增长，而经历高温后，强度有所降低，但经历了1400℃处理后仍能保持结构的完整。而耐久性的研究也表明磷酸镁水泥具有较好的抗冻融循环和抗浸泡性能。通过对强度、温度对基材性能的影响以及耐久性的研究分析，表明磷酸镁水泥是一种理想的固化基材。
由于Cs和Sr是中低放射性废物中最常见且危害最大的两种放射性核素，通过掺加Cs和Sr研究了Cs和Sr对磷酸镁水泥水化和硬化的影响，磷酸镁水泥对Cs和Sr的吸附性能、含核素固化体的浸出率以及耐久性、以及Cs和Sr在磷酸镁水泥中的存在状态。掺加Cs和Sr均对磷酸镁水泥的抗压强度造成影响，造成了磷酸镁水泥强度的下降。磷酸镁水泥对Cs和Sr均具有较好的吸附性能，尤其对Sr吸附率高达97.72%。掺加Cs的固化体42d浸出率和累计浸出分数低至5.47×10-5cm·d-1和2.81×10-3cm，而掺加Sr的固化体Sr的42d浸出率和累计浸出分数可达2.85×10~(-5)cm·d~(-1)和5.92×10~(-3)cm。Cs对磷酸镁水泥早期水化影响较小，而Sr的影响较大，Sr的掺入降低了磷酸镁水泥的水化热，延缓了水化。Cs和Sr在固化体中主要以难溶的MgCsPO4·6H_2O和SrHPO_4形式存在，使其固化体浸出率大幅降低。
放射性焚烧灰是目前固化处理的难点。本文采用磷酸镁水泥固化模拟放射性焚烧灰。首先进行包容量研究，其次是对固化体的性能进行分析。通过强度分析，磷酸镁水泥对模拟焚烧灰的最大包容量可以达到60wt%。水化热分析表明模拟放射性焚烧灰掺量越大，固化体的水化热越低，导致水化进程有较大延缓。固化体Cs的浸出率为1.7×10-4cm·d~(-1)，累计浸出分数为0.15cm；Sr的浸出率为1.1×10-4cm·d~(-1)，累计浸出分数为0.015cm。对固化体的流动度，抗冲击性能、抗冻融性能和抗浸泡性能研究也表明了其完全满足固化体性能指标要求。
本研究表明，磷酸镁水泥对于中低放射性废物具有良好的固化性能。主要原因是由于核素与其它反应物形成了难溶的磷酸盐矿物，同时辅以磷酸镁水泥水化物的包裹作用，可快速将核素固定在固化体中，具有较大的废物包容量。因此磷酸镁水泥是一种理想的中低放射性废物固化基材。
Cement solidification process has significant advantage when applied in thedisposal of medium and low level radioactive wastes. Compared with othersolidification process, technology and equipment for cement solidification process isvery simple and low cost, solidified form also has good durability. So, cementsolidification process has been widely applied in storage and transportation of mediumand low level radioactive wastes. Traditional cement solidification technology hasmany disadvantages, such as high water to cement ratio, high nuclei leaching rate, lowsolidified form strength and etc. Traditional cement must cure under high pH valueenvironment，wastes need treatment previously. The setting time and strength ofcement may affected by PO43-, BO33-, Zn, Sn. Due to the disadvantages above,traditional cement solidification process has low wastes loading, which means morespace must remain to the storage, and the transportation of wastes is also a big problem.Therefore, the selection of new type cement for medium and low level radioactivewastes is necessary，the target of selection is improve the performance of the solidifiedform, improve the loading capacity and speed the solidification process, and finally getsolidified form with better durability, promote cement solidification process in the fieldof treatment and disposal of nuclear waste. Considering the characteristics ofmagnesium phosphate cement (MPC), magnesium phosphate cement was selected asmatrix material in this study for solidifying medium and low level radioactive waste,and solification of medium and low level radioactive incineration ash was also studied.
First of all, the related performances of magnesium phosphate cement which infavor of medium and low level radioactive wastes solidification were studied. In orderto select suitable matrix material, three kinds of phosphate were chose to preparationmagnesium phosphate cement; the effects of mix ration to the strength were alsostudied. Considering the preparation of solidified form of magnesium phosphatecement may be affected by the very low temperature, the strength development ofMPC was studied by curing under-20℃.The properties of MPC after various hightemperature treatments were also studied. Durability is also an important factor ofsolidified form, freezing and thawing test and soaking test were used to investigate thedurability of samples. Results show MPC prepared by ammonium dihydrogenphosphate has highest strength, the latter is MPC prepared by potassium dihydrogen phosphate, diammonium hydrogen phosphate is the worst. M/P plays a key role to thestrength of MPC, followed by effects of borax, particle size of magnesium oxide hasminimal effection. Strength of magnesium phosphate cement has been able to achievegrowth under low temperature conditions. Magnesium phosphate cement-basedmaterials have superior high-temperature performance, the structure of cement stillmaintain integrity even at up to1400℃, volume of samples will reduce under differenttemperature treatment, structural collapse did not occur whthin the full temperaturerange. Durability studies show that magnesium phosphate cement has good resistanceto freeze-thaw and soaking test. The results indicate magnesium phosphate cement isan ideal matrix material.
Secondly, because Cs and Sr are two of the most common and dangerest nuclei ofmedium and low level radioactive wastes, the solidification performance of MPC byadding Cs and Sr was studied. The affections of Sr and Cs addition to the strength ofMPC were studied, as well the hydration of MPC. The adsorption performance ofmagnesium phosphate cement to Cs, Sr was also studied. The durability and theexistence state of Cs and Sr in MPC were also investigated. Adding Cs and Sr causethe decline in the strength of MPC. Magnesium phosphate cement have betterperformance on adsorption Sr, absorption rate for Sr is up to97.72%. The42d leachingrates and cumulative leaching factor of solidified form with Cs are5.47x10-5cm·d-1and2.81x10-3cm respectively, and those of Sr are2.85x10-5cm·d-1and5.92x10-3cmrespectively. Sr addition reduces the hydration heat of hydration of magnesiumphosphate cement, slow hydration process, but those of Cs is not so significant.Cs andSr are mainly as MgCsPO4·6H2O and SrHPO4existed in the solidified form, so theleaching rates are significantly lower than other cement system,especially at the earlyleaching test.
Immobilization of radioactive incineration ash is a difficult in wastes diaposal.Magnesium phosphate cement was chosed to immbilizaton for simulated radioactiveincineration ash. The loading capacity of solidified form was studied, and theperformance of solidified form was also investigated. Through analysis of compressivestrength, maximum loading capacity of solidified form can reach60wt%. Hydrationheat analysis indicates with higher simulated radioactive incineration ash, the lowerhydration heat of solidified form can be found, caused the hydration process delay. Theleaching rate and cumulative leaching rate of solidified form can reach1.7×10-4cm·d-1and0.15cm for Cs,1.1×10-4cm·d~(-1)and0.015cm for Sr. fluidity of pastes, impact resistance, freezing and thawing resistance and anti soaking are fully met performancerequirements of solidified form.
This study showed that magnesium phosphate cement has good performance forsolidification of medium and low level radioactive waste. With the formation ofinsoluble phosphate mineral, and encapsulating with the hydration products of MPC,radioactive ions can be quickly fixed in the solidified form, and the final form has gooddurability. MPC is an ideal matrix material for medium and lowlevel radioactivewastes solidification.
引文
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