Новые сорбционные методы удаления цезия и актинидов из кислых сред тема диссертации и автореферата по ВАК РФ 05.17.02, кандидат технических наук Тодд Терри Аллен

• Тодд Терри Аллен
• кандидат технических наук
• 2005

Оглавление диссертации кандидат технических наук Тодд Терри Аллен

Table of Contents

INTRODUCTION

1. LITERATURE REVIEW

1.1 Review of Literature related to separation of Cesium by ion Exchange

1.1.1 Review of Literature Related to Ammonium Molybdophosphate

as a Cesium Exchanger

1.1.2 Review of Literature Related to Crystalline Silicotitanate

(IONSIV IE- 911) as a Cesium Ion Exchanger

1.1.3 Review of Literature Related to Hexacyanoferrates as a Cesium Ion . Exchanger

1.1.4 Review of Literature Related to Other Types of Cesium Ion

Exchangers

1.2 Review of Literature related to separation of Actinides by Extraction chromatography

1.3 Statement of the problem

2. EXPERIMENTAL

2.1 Experimental Description of Cesium Ion Exchange Testing

2.1.1 Feed Compositions of INEEL Simulated Tank Waste

2.1.2 Feed Compositions of Actual INEEL Tank Waste

2.1.3 Analytical methods

2.1.4 Characteristics of AMP-PAN/SF02 Sorbent

2.1.5 Characteristics of IONSIV IE-911 (CST) Sorbent

2.1.6 Equilibrium Batch Distribution Coefficient (Kd)

2.1.7 Experimental Methods for Equilibrium Batch Distribution-.

Coefficient Measurement

2.1.8 Experimental Procedure for Small-Scale Column Tests using

AMP-PAN and CST with Simulated Waste Solutions

2.1.9 Experimental Procedure for Small-Scale Column Tests using

AMP-PAN and CST with Actual Waste Solutions

2.1.10 Experimental Procedure for Intermediate-Scale Column Tests using . AMP- PAN

2.1.11 Experimental Procedure for Intermediate-Scale Column Tests using . CST

2.2 Experimental description of solid phase extradant synthesis and testing

2.2.1 Synthesis of PAN-based solid phase extractants

2.2.2 Batch Equilibrium Comparison Study of CMPO-PAN and

TRU-Resin®

2.2.3 CMPO-PAN Acid Dependency Batch Equilibrium Studies

2.2.4 Investigation of Elution Methods for CMPO-PAN

3. RESULTS AND DISCUSSION

3.1 Results and Discussion of Cesium Ion Exchange Testing

3.1.1 Equilibrium Isotherm Determinations for AMP-PAN and CST

3.1.2 Investigation of the Effects of H+,Na, and K on Cs Distribution . Coefficients for AMP-PAN and CST

3.1.3 Investigation on the Sorption of Plutonium, Americium and Mercury . with AMP-PAN and CST

3.1.4 Results of Small-Scale Column Tests using AMP-PAN and CST to . Remove Cesium from INEEL Simulated Tank Waste

3.1.5 Results of Small-Scale Column Tests using AMP-PAN and CST to .

<4 Remove Cesium from INEEL Actual Tank Waste

3.1.6 Results of Intermediate-Scale Column Testing using AMP-PAN to . Remove Cesium from INEEL Simulated Tank Waste

3.1.7 Results of Intermediate-Scale Column Testing using IONSIV IE-911 . (CST) to Remove Cesium from INEEL Simulated Tank Waste

3.1.8 Thermometric Gravitational Analysis/Differential Temperature

Analysis

3.2 Technological Flowsheets and Application to INEEL HLW

3.3 Summary of Cesium Ion Exchange Results with AMP-PAN and CST for

INEEL Acidic Tank Waste

^ 3.4 Investigation of PAN-Based solid phase extractants for Separation of

Actinides from simulated tank waste and analytical samples

3.4.1 Physical Characterization of Solid Phase Extractants

3.4.2 Results of Batch Equilibrium Studies with CMPO-PAN and

TRU- Resin®

3.4.3 Investigation of Equilibrium acid dependency for CMPO-PAN

in HN03 and HC1

3.4.4 Investigation of Elution Methods for CMPO-PAN

3.4.5 Investigation of Uranium Uptake on CMPO-PAN

3.4.6 Investigation of Fe(III) Uptake on CMPO-PAN

" CONCLUSIONS

REFERENCES

Введение диссертации (часть автореферата) на тему «Новые сорбционные методы удаления цезия и актинидов из кислых сред»

INTRODUCTION

The Idaho Nuclear Technology and Engineering Center (INTEC), located at the Idaho National Engineering and Environmental Laboratory (INEEL), was built in the early 1950's to reprocess government-owned, spent nuclear fuel. The fuel assemblies were completely dissolved and highly-enriched uranium was recovered from the resulting acidic liquid using modified PUREX and REDOX-type solvent extraction processes. Liquid raffinates were stored in single-shell stainless-steel tanks, as acidic liquids, until they were solidified in a fluidized bed calciner. Incidental wastes, primarily from solvent washing activities, evaporator bottoms and decontamination activities were also stored in the underground storage tanks. Incidental wastes were collected in separate tanks from the extraction raffinates. The incidental wastes typically contained a relatively high amount of sodium and potassium, and are difficult to calcine in a fluidized bed because the alkali metals melt and form agglomerates. The incidental wastes were blended with extraction process raffinates prior to calcination to deplete their inventory. A total of eleven 1100 m3 liquid storage tanks were built and are contained in underground concrete vaults.

In 1992, the Department of Energy halted reprocessing activities at the INEEL and the primary focus of the facility changed to 1) interim storage of spent nuclear fuel, 2) management of liquid and solid wastes and 3) decommissioning of facilities. In this same year, the United States Environmental Protection Agency and the Idaho Department of Health and Welfare filed a Notice of Noncompliance (NON) contending that the underground storage tanks do not meet secondary containment

requirements as set forth in United States Federal Regulations. In 1995, a Settlement Agreement (court order) was signed by the Department of Energy, the Navy and the State of Idaho, which allowed spent nuclear fuel shipments to Idaho to continue only if liquid tank waste and calcine were treated and eventually removed from the State of Idaho. The agreement requires all liquid waste to be removed from the underground storage tanks_by 2012. There are currently approximately 4000 m3 of acidic highly-radioactive liquid waste stored at the INEEL.

Development activities have been underway to evaluate a number of treatment options for the liquid wastes. The primary focus of the development efforts has been directed toward the use of separation technologies to remove the radionuclides from the waste solutions. The length of the half-lives associated with the radionuclides present in radioactive wastes is the basis for concern to the environment and human health factors. The half-lives of the actinides (Pu, U, Am, and Np) range from a few hundred years to several thousand years or more. The presence of these long-lived elements in significant concentrations presents a challenge to the management of radioactive wastes. Present methods for storage of the liquid radioactive wastes are not likely to be effective for the period of time required for the actinides to decay to low activities. Therefore, long-term immobilization of these elements must be accomplished to allow final disposal in a geological repository. The current approach in the United States and around the world is to secure these elements in immobilized forms such as vitrified glass. This approach appears effective and is among the best options for the disposal of radioactive wastes at this time.

The half-lives of other radionuclides of concern, however, are much shorter. The half-lives of the fission products, 90Sr and 137Cs, are 29 years and 30 years, respectively. In general, it can be stated that ten half-lives of these isotopes (approximately 300 years) is the length of time required for these elements to be reduced to activities which are below levels of concern. It is likely that current technology could yield an engineered containment for these elements which would provide a secure disposition of these elements without the cost of vitrification and deep geologic disposal. The INEEL is evaluating different approaches to management of these fission products which include separation and immobilization in glass, for shipment to the U.S. high-level waste repository, or separation and immobilization in concrete with disposal at the Waste Isolation Pilot Plant (WIPP).

Regardless of the final disposition of the fission products, it is clear that the separation of these long-lived components from the waste residing in the current storage facilities must be accomplished in an efficient and timely manner. Human safety, environmental protection, and cost of treatment must be considered with primary importance during the evaluation of waste treatment options. A primary goal of the INEEL is to reduce the actinide and fission product activities to levels which will allow the disposal of the majority of the radioactive waste as U. S. Nuclear Regulatory Commission (NRC) low-level waste (LLW). The resulting reduction in the amount of waste requiring disposal as a high-level waste (HLW) in a geological repository would significantly reduce disposal costs. Specific criteria for NRC Class A, B, and C LLW are given in Table 1. Reduction of the activity to .Class A LLW limits is the most desirable option. This would require removal efficiencies of approximately 98,1%,

99,5%, and 99,98% for the TRUs, 137Cs, and 90Sr, respectively for 1NEEL liquid waste solutions.

Table 1. U. S. Nuclear Reglatory Commission (NRC) low-level waste classifications

Component Class A LLW Class B LLW Class C LLW

TRUs lOnCi/g 100 nCi/g 100 nCi/g

Sr-90 0,04 Ci/m3 150 Ci/m3 7000 Ci/m3

Cs-137 1 Ci/m3 44 Ci/m3 4600 Ci/m3

Two technological approaches have been developed for the separation of radioactive elements from the acidic liquid tank waste. The first involves the decontamination of the tank waste from the major radioactive elements (actinides, lanthanides, cesium and strontium). The second approach involves the separation of only cesium, then grouting of the remaining waste. In the first approach, the cesium can be removed in the first process, by ion exchange, thus reducing shielding and handling requirements in the downstream actinide and strontium separation processes, such as the transuranium extraction process (TRUEX) and the strontium extraction process (SREX), respectively. The separated radionuclides would be vitrified and sent to the high-level' waste repository. In the second approach, only the cesium would be separated from the waste, by ion exchange, and the remaining liquid would be grouted and sent to the Waste Isolation Pilot Plant as remote-handled transuranic waste.

Development and operation of treatment processes for highly-radioactive waste are dependent on reliable, simple analytical methods. Highly effective analysis methods currently exist, but are reliant on extremely complicated and sensitive instrumentation, such as ICP-MS. The INEEL is interested in developing methods to separate actinides or other radionuclides allowing for simple radiometric counting methods to be

employed. To this end, separation of actinides from other elements is an essential part of this scheme. The current method for separation of actinides is the use of commercial extraction chromatography resins, such as TRU-Resin , produced by Eichrom Technologies, Darian, IL, USA. Extraction chromatography is a method that combines the high selectivity of liquid-liquid extraction, with the ease of operation of column chromatography. These materials consist of an extractant, dissolved in an organic diluent, and sorbed into the pores of an inert matrix bead. The amount of extractant that can be placed on a bead is limited by pore volume and solubility of the extractant in the diluent. Stable elements present in the waste stream (such as Fe or Zr) are present in much higher masses than the actinides, and tend to load the extraction chromatography resins to capacity, limiting their effectiveness. A new type of actinide sorbent, with significantly higher capacity would be beneficial to the analysis of radioactive elements at INEEL.

Scientific Novelty of This Research

The scientific novelty of this work is summarized as follows:

1. A new granular sorbent, based on ammonium molybdophosphate -polyacrylonitrile (AMP-PAN), has been shown to be effective at removing Cs from acidic radioactive waste.

2. A new inorganic granular sorbent, crystalline silicotitanate, has been shown to be effective at removing Cs from acidic radioactive waste.

3. A new class of solid phase extradants has been invented using PAN as the matrix and classical organic extradants. Successful immobilization of

soluble extractants rather than insoluble sorbents in PAN matrix has been demonstrated.

4. CMPO and Aliquat 336 extractants have been shown to have excellent extraction properties while incorporated in PAN matrix.

Practical Importance of This Research

The feasibility of using two new ion exchange sorbents for separation of Cs from acidic HLW has been demonstrated. Separation of Cs from HLW reduces the need for shielding of downstream processes and waste containers. Separation of Cs allows for more effective management of this highly-radioactive, but short half-life element. New solid-phase extractants can be prepared with up to 30 wt% extractant, which is much higher than conventional extraction chromatography resins. New solid-phase extractants could improve analytical separation procedures/methods. CMPO-PAN has a higher affinity for Am and Pu as well as significantly higher capacity for extracted metals than TRU-Resin®. Aliquat 336-PAN has been shown to effectively separate Pu from Am in acidic solutions, as well as extract Tc over a wide pH range.

Goals of This Research

1. Investigate the physical characteristics and chemical separation properties of AMP-PAN and CST sorbents for the separation of cesium from INEEL simulated and actual acidic tank waste. Provide a technical basis for engineering design studies related to the separation of cesium from INEEL tank waste.

Develop a synthetic method of preparing solid phase sorbents using organic extractants, such as CMPO and Aliquat 336 and characterize the physical properties of the sorbents.

Determine the effectiveness and capacity of solid phase sorbents, based on the extractants CMPO and Aliquat 336 at separating actinides from acidic media. Compare the effectiveness of the new PAN-based sorbent to commercial extraction chromatography resins.

Conclusions

1. A simple method for the incorporation of organic extractants into a PAN matrix have been developed. Two new sorbents, based on CMPO and Aliquat-336 have been prepared using this method. This method can be expanded to other classes of organic extractants. Preparation methods and possible applications of these sorbents have been patented.

2. The physical structure of sorbent particles was investigated. Extraction of actinides as a function of acid concentration and in the presence of stable metals was studied. These sorbents were tested for extraction of actinides from acidic radioactive waste. CMPO-PAN sorbent showed better extraction properties for actinides than commercial CMPO-based TRU-Spec® extraction chromatography resin.

3. Two new granular sorbents for cesium removal from acidic media, AMP-PAN and CST, have been investigated. Cesium equilibrium isotherms, the effects of competing ions on cesium sorption, and the sorption of Am, Pu and Hg were investigated.

3.

4. Cesium sorption in fixed-bed ion exchange columns at different scales was studied, using actual and simulated INEEL radioactive waste. Testing was performed on 1,5 liter samples of actual waste and up to 450 L of simulated waste. Approximately 1500 bed volumes of INEEL waste can be processed before initial breakthrough using AMP-PAN while only about 100 bed volumes for CST. Column performance was predicted using computer modeling with less than 10% error.

5. Results from AMP-PAN and CST testing were used as the basis for an engineering feasibility study by the INEEL High-Level Waste program. The Department of Energy (DOE) is considering cesium ion exchange by these sorbents as one of the potential treatment methods for radioactive tank waste.

Recognition and Publications Related to This Research

This research has resulted in one United States Patent and an additional three United States Patents have been filed and are pending. This research has been published in 14 peer-reviewed scientific journals. Six presentations have been made at international technical conferences and seven presentations made at national technical conferences in the United States.

Structure and Volume of Dissertation

The dissertation consists of an introduction, literature review, experimental section, four results and discussion sections, conclusions and the list of 154 references. The dissertation is written on 118 typewritten pages and contains 15 tables and 31 figures.

Заключение диссертации по теме «Технология редких, рассеянных и радиоактивных элементов», Тодд Терри Аллен

CONCLUSIONS

1. A simple method for the incorporation of organic extractants into a PAN matrix have been developed. Two new sorbents, based on CMPO and Aliquat-336 have been prepared using this method. This method can be expanded to other classes of organic extractants. Preparation methods and possible applications of these sorbents have been patented.

2. The physical structure of sorbent particles was investigated. Extraction of actinides as a function of acid concentration and in the presence of stable metals was studied. These sorbents were tested for extraction of actinides from acidic radioactive waste. CMPO-PAN sorbent showed better extraction properties for actinides than commercial CMPO-based TRU-Resin® extraction chromatography resin.

3. Two new granular sorbents for cesium removal from acidic media, AMP-PAN and CST, have been investigated. Cesium equilibrium isotherms, the effects of competing ions on cesium sorption, and the sorption of Am, Pu and Hg were investigated.

4. Cesium sorption in fixed-bed ion exchange columns at different scales was studied, using actual and simulated INEEL radioactive waste. Testing was performed on 1,5 liter samples of actual waste and up to 450 L of simulated waste. Approximately 1500 bed volumes of INEEL waste can be processed before initial breakthrough using AMP-PAN while only about 100 bed volumes for CST. Column performance was predicted using computer modeling with less than 10% error.

Results from AMP-PAN and CST testing was used as the basis for an engineering feasibility study by the INEEL High-Level Waste program. The Department of Energy (DOE) is considering cesium ion exchange by these sorbents as one of the potential treatment methods for radioactive tank waste.

Список литературы диссертационного исследования кандидат технических наук Тодд Терри Аллен, 2005 год

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