CN103165206B - Thorium uranium mixed oxide ceramic microsphere preparation method - Google Patents

Thorium uranium mixed oxide ceramic microsphere preparation method Download PDF

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CN103165206B
CN103165206B CN201110421836.5A CN201110421836A CN103165206B CN 103165206 B CN103165206 B CN 103165206B CN 201110421836 A CN201110421836 A CN 201110421836A CN 103165206 B CN103165206 B CN 103165206B
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thorium
drying
calcining
colloidal sol
tho
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CN103165206A (en
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尹荣才
刘小龙
左国平
卢长先
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Nuclear Power Institute of China
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Nuclear Power Institute of China
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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
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    • Y02E30/30—Nuclear fission reactors

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Abstract

The invention belongs to a kind of manufacture method of nuclear fuel, specifically thorium uranium mixed oxide ceramic microsphere preparation method.Method of the present invention is gelling process in adopting, and with acid deficient uranyl nitrate solution and thorium nitrate for raw material, through colloidal sol preparation, dispersion gelling, washing, drying and calcining and reduction sintering process, prepares the ThO that diameter is 0.05 ~ 0.20mm 2-UO 2microballoon.This ThO 2-UO 2microballoon has smooth surface, spherical good, interior solid, thorium are evenly distributed, density is greater than 96.8%TD outstanding advantages; Method itself is simple, can prepare the thorium uranium mixed oxide ceramic microsphere of different thorium content.

Description

Thorium uranium mixed oxide ceramic microsphere preparation method
Technical field
The invention belongs to a kind of manufacture method of nuclear fuel, specifically thorium uranium mixed oxide ceramic microsphere preparation method.
Background technology
Neutron-absorption cross-section due to thorium fuel is 3 times of uranium fuel, the conversion efficiency ratio of thorium in thermal-neutron reactor 238u is high, adds in uranium fuel simultaneously 232th, is equivalent to add burnable poison, can charge under identical heap level of control more, thus extends core life.The utilization of thorium fuel can also make the radial power distribution of reactor core flatten, thus makes reactive control simple and easy.Therefore, (Th, U) O is adopted 2ceramic fuel is one of effective way extending lifetime of reactor core.
For the preparation of thorium uranium mixed oxide ceramic microsphere, mainly adopt sol-gal process abroad.U.S.'s Oak Ridge National Laboratory adopts oxide sol to prepare thorium uranium mixed oxide microballoon in early days, as Laboratory studies of sol-gel processes at the Oak Ridge National Laboratory " ThO described in (O RNL-TM-1980,1967) 2-UO 2the preparation method of colloidal sol is: (1) co-precipitation-peptization, (2) ThO 2colloidal sol and UO 2colloidal sol simply mixes, ThO 2-UO 3the preparation method of colloidal sol is: (1) co-precipitation-peptization-concentration method, and (2) are obtained by uranyl nitrate solution peptization thorium dioxide precipitation.(3) by UO 3join ThO 2obtained in colloidal sol, (4) solvent extraction.In this preparation method, the gelling of colloidal sol adopts the moisture in extraction colloidal sol to realize, and colloidal sol preparation process is complicated, and process conditions are harsh, control difficulty is large.And for example: " Preliminary development of internal gelation flowsheets for preparing (Th, U) O 2spheres " have employed in (ORNL/TM-7280,1981) and be similar to interior gelling and prepare UO 2the method of ball prepares (Th, U) O of Th/U=3 2microballoon, to add in thorium nitrate and acid deficient uranyl nitrtate mixed solution in ammoniacal liquor part and, then add urea (Urea) and urotropine (HMTA) is mixed with colloidal sol.This method is conducive to preparing good (Th, the U) O of surface quality 2microballoon, but this colloidal sol preparation method easily produces precipitation when uranium content is high.Japan Atomic can the H. Tel etc. of graduate Shigeru YAMAGISHI etc. and atomic energy science institute of Ege university of Turkey at " Journal of Nuclear Science and Technology " 23 (9), " Production of (Th, the U) O of pp.794 ~ 801 (September 1986) 2microspheres with Uranium Content of 0 ~ 35% by Sol-Gel Process Using CCl 4as Gelation Media " and " the Investigation of production conditions of ThO of " Journal of Nuclear Materials " 256 (1998) 18-24 2-UO 3microspheres via the sol-gel process for pellet type fuels " in describe and obtain ThO with ammonia neutralization thorium uranium mixed nitrate solution 2-UO 3colloidal sol adopts outer gelling process to prepare gel micro-ball, but this colloidal sol preparation method is comparatively complicated, wayward.
Summary of the invention
The object of the present invention is to provide a kind of simple thorium uranium mixed oxide ceramic microsphere preparation method, the method can prepare the thorium uranium mixed oxide ceramic microsphere of different thorium content.
Technical scheme of the present invention is as follows:
Thorium uranium mixed oxide ceramic microsphere preparation method, comprises colloidal sol preparation, dispersion gelling, washing, drying and calcining and reduction sintering, it is characterized in that: the concrete steps of described thorium uranium mixed oxide ceramic microsphere preparation method are as follows:
step onecolloidal sol preparing process: thorium nitrate is joined in acid deficient uranyl nitrate solution and dissolve, the wherein NO of acid deficient uranyl nitrate solution 3 -/ U (mol ratio)=1.5 ~ 1.8; Th/ (Th+U) (mol ratio)=0.1 ~ 0.5; It is 2.31mol/L that gained mixed solution adds the concentration sum that deionized water is adjusted to uranium and thorium, then this mixed solution is cooled to 0 DEG C ~ 5 DEG C, slowly adds urea and urotropine, be mixed with the colloidal sol of homogeneous transparent, wherein the material of urea 'sthe material of amount and uranium and thorium 'sthe ratio of amount sum is 1.3 ~ 1.8, the material of urotropine 'sthe material of amount and uranium and thorium 'sthe ratio of amount sum is 1.3 ~ 2.2;
step 2dispersion gelatinizing process: be distributed in the gelation media 2-Ethylhexyl Alcohol of 60 DEG C ~ 95 DEG C by diverting device by colloidal sol, gelling becomes gel ball;
step 3washing process: the mixed solution of gel ball ammoniacal liquor and ethanol is washed, NH in cleansing solution 4oH concentration is 0.5 ~ 3.0mol/L, C 2h 5the percent by volume of OH is 50%, and washing times is 3 ~ 4 times, at every turnwash time is 20 ~ 50min;
step 4drying and calcining process :gel ball after washing is placed in drying calciner drying and calcining, makes it to change into ThO 2-UO 3microballoon, adds the humidity of water management drying and calcining process, and wherein amount of water is 1000 ml ~ 2000ml, and gel ball drying and calcining heating schedule is: rise to 80 DEG C at 90min ~ 120min from room temperature, then rises to 90 DEG C at 60min ~ 80min; Then in 90min ~ 120min, 150 DEG C are risen to, insulation 90min ~ 180min; 200 DEG C are risen to subsequently, insulation 50min ~ 80min at 50min ~ 80min; 350 DEG C are risen to again, insulation 60min ~ 150min at 50min ~ 80min;
step 5reduction sintering process: by the ThO after drying and calcining 2 -UO 3 microballoon, is carry out reduction sintering under the hydrogen atmosphere of 1200 DEG C ~ 1500 DEG C in sintering temperature, obtains the fine and close ThO that diameter is 0.05 ~ 0.2mm 2 -UO 2 ceramic microsphere.
Effect of the present invention is: preparation method of the present invention does not have rigors to process equipment, simple, is controlled the gelling balling property of colloidal sol, the ThO of preparation by the proportioning controlling urea (Urea) and urotropine (HMTA) 2-UO 2microsphere features smooth surface, spherical good, interior solid, thorium are evenly distributed; ThO 2-UO 2microsphere diameter is 0.05 ~ 0.20mm, density 96.8%T.D ~ 98.3%T.D.
Embodiment
Thorium uranium mixed oxide ceramic microsphere preparation method of the present invention: be add thorium nitrate in acid deficient uranyl nitrate solution, then adds urea and urotropine is mixed with colloidal sol.Be distributed in the 2-Ethylhexyl Alcohol of heat by diverting device by colloidal sol, gelling becomes gel ball.The gel ball obtained adopts the mixed solution washing of ammoniacal liquor and ethanol, removes NO wherein 3 -deng solvend.Then in high temperature oven, carry out drying and calcining, transform into ThO 2-UO 3microballoon.ThO 2-UO 3microballoon, through reduction sintering, obtains fine and close ceramic ThO 2-UO 2microballoon.
Concrete preparation process is as follows:
Step one colloidal sol is prepared: in acid deficient uranyl nitrate solution, add thorium nitrate, adding deionized water to liquor capacity after thorium nitrate has dissolved is 50ml, then mixed solution is cooled to less than 5 DEG C, slowly adds urea and urotropine, limit edged stirs, and is mixed with the colloidal sol of homogeneous transparent; Wherein the ratio of thorium is: Th/ (Th+U) (mol ratio)=0.1 ~ 0.5; The NO of acid deficient uranyl nitrate solution 3 -/ U (mol ratio)=1.5 ~ 1.8; It is 2.31mol/L that gained mixed solution adds the concentration sum that deionized water is adjusted to uranium and thorium, the wherein material of urea 'sthe material of amount and uranium and thorium 'sthe ratio of amount sum is 1.3 ~ 1.8, the material of urotropine 'sthe material of amount and uranium and thorium 'sthe ratio of amount sum is 1.3 ~ 2.2;
Step 2 dispersion gelling: be distributed in the gelation media 2-Ethylhexyl Alcohol of 60 DEG C ~ 95 DEG C by diverting device by colloidal sol, gelling becomes gel ball;
Step 3 is washed: washed by the mixed solution of gel ball ammoniacal liquor and ethanol, NH in cleansing solution 4oH concentration is 0.5 ~ 3.0mol/L, C 2h 5the percent by volume of OH is 50%, and washing times is 3 ~ 4 times, at every turnwash time is 20 ~ 50min;
Step 4 drying and calcining: by the gel ball drying and calcining in high temperature oven after washing, transform into ThO 2-UO 3microballoon; Add the water of 1000ml ~ 2000 in drying calciner, control the humidity in drying and calcining process; Gel ball drying and calcining heating schedule is: in 90 ~ 120min, rise to 80 DEG C from room temperature, then in 60 ~ 80min, rise to 90 DEG C; Then in 90 ~ 120min, 150 DEG C are risen to, insulation 90 ~ 180min; 200 DEG C are risen to subsequently, insulation 50 ~ 80min in 50 ~ 80min; 350 DEG C are risen to again, insulation 60 ~ 150min in 50 ~ 80min;
Step 5 reduction sintering: by the ThO after drying and calcining 2 -UO 3 microballoon, is carry out reduction sintering under the hydrogen atmosphere of 1200 DEG C ~ 1500 DEG C in sintering temperature, obtains the fine and close ThO that diameter is 0.05 ~ 0.2mm 2 -UO 2 ceramic microsphere.
Below in conjunction with embodiment, method of the present invention is further described:
embodiment 1
step one colloidal sol is prepared:get acid deficient uranyl nitrate solution ([U]=630g/l, NO 3 -/ U mol ratio=1.80) 39.3ml, add thorium nitrate (Th (NO 3) 44H 2o) 6.4g(Th/ (Th+U)=0.1).Adding deionized water to liquor capacity after thorium nitrate has dissolved is 50ml.Mixed solution is cooled to less than 5 DEG C, slowly adds 9.0g Urea and 21.0g HMTA(Urea, HMTA/U mol ratio=1.3), limit edged stirs, and obtains the colloidal sol of homogeneous transparent.
step 2 dispersion gelling:disperseed by the dispersing head in colloidal sol 0.2mm aperture, the colloidal sol that dispersion is formed drips and enters in the 2-Ethylhexyl Alcohol gelation media of 60 DEG C, obtained Wet Gel Microsphere;
step 3 is washed:by the 0.5mol/l ammonia scrubbing 4 time of gel micro-ball containing 50vol% ethanol, wash 20min at every turn,
step 4 drying and calcining:by the gel ball drying and calcining in high temperature oven after washing, add water in high temperature oven 1000ml, and drying and calcining heating schedule is: in 90min, rise to 80 DEG C from room temperature, then rise to 90 DEG C in 60min, then rises to 150 DEG C in 90min, insulation 120min; 200 DEG C are risen to subsequently, insulation 80min in 80min; 350 DEG C are risen to again, insulation 60min in 50min;
step 5 reduction sintering:by the ThO after drying and calcining 2-UO 3microballoon reduces sintering in a hydrogen atmosphere, obtains the ceramic of compact ThO that diameter is 0.05 ~ 0.2mm 2-UO 2microballoon, sintering temperature is 1500 DEG C, and the density of microballoon is 98.3%T.D.
embodiment 2
step one colloidal sol is prepared:get acid deficient uranyl nitrate solution ([U]=610g/l, NO 3 -/ U mol ratio=1.60) 31.5ml, add thorium nitrate (Th (NO 3) 44H 2o) 19.1g(Th/ (Th+U)=0.3).Adding deionized water to liquor capacity after thorium nitrate has dissolved is 50ml.Mixed solution is cooled to less than 5 DEG C, slowly adds 10.4g Urea and 29.9g HMTA(Urea/ (U+Th) mol ratio=1.5, HMTA/ (U+Th) mol ratio=1.85), limit edged stirs, and obtains the colloidal sol of homogeneous transparent.
step 2 dispersion gelling:disperseed by the dispersing head in colloidal sol 0.2mm aperture, the colloidal sol that dispersion is formed drips the 2-Ethylhexyl Alcohol gelation media entering 75 DEG C, obtained Wet Gel Microsphere.
step 3 is washed:by the 0.5mol/l ammonia scrubbing 3 time of gel micro-ball containing 50vol% ethanol, wash 40min at every turn,
step 4 drying and calcining:by the gel ball drying and calcining in high temperature oven after washing, add water in high temperature oven 1500ml, and drying and calcining heating schedule is: in 100min, rise to 80 DEG C from room temperature, then in 80min, rise to 90 DEG C, then in 120min, rises to 150 DEG C, insulation 90min; 200 DEG C are risen to subsequently, insulation 80min in 60min; 350 DEG C are risen to again, insulation 100min in 60min.
step 5 reduction sintering:by the ThO after drying and calcining 2-UO 3microballoon reduces sintering in a hydrogen atmosphere, obtains the ceramic of compact ThO that diameter is 0.05 ~ 0.2mm 2-UO 2microballoon, microballoon sintering temperature is 1300 DEG C, and the density of microballoon is 97.9%T.D.
embodiment 3
step one colloidal sol is prepared:get acid deficient uranyl nitrate solution ([U]=620g/l, NO 3 -/ U mol ratio=1.50) 22.1ml, add thorium nitrate (Th (NO 3) 44H 2o) 31.9g(Th/ (Th+U)=0.5).Adding deionized water to liquor capacity after thorium nitrate has dissolved is 50ml.Mixed solution is cooled to less than 5 DEG C, slowly adds 12.5g Urea and 35.6g HMTA(/ (U+Th) mol ratio=1.8, Urea, HMTA/ (U+Th) mol ratio=2.2), limit edged stirs, and obtains the colloidal sol of homogeneous transparent;
step 2 dispersion gelling:the dispersing head in colloidal sol 0.2mm aperture disperses, and the colloidal sol that molten dispersion is formed drips the 2-Ethylhexyl Alcohol gelation media entering 95 DEG C, obtained Wet Gel Microsphere;
step 3 is washed:by the 0.5mol/l ammonia scrubbing 4 time of gel micro-ball containing 50vol% ethanol, wash 50min at every turn,
step 4 drying and calcining:by the gel ball drying and calcining in high temperature oven after washing, add water in high temperature oven 2000ml, and drying and calcining heating schedule is: in 120min, rise to 80 DEG C from room temperature, then in 70min, rise to 90 DEG C, then in 100min, rises to 150 DEG C, insulation 180min; 200 DEG C are risen to subsequently, insulation 50min in 50min; 350 DEG C are risen to again, insulation 150min in 80min;
step 5 reduction sintering:by the ThO after drying and calcining 2-UO 3microballoon reduces sintering in a hydrogen atmosphere, obtains the ThO that diameter is 0.05 ~ 0.2mm 2-UO 2microballoon, microballoon sintering temperature is 1200 DEG C, and the density of microballoon is 96.8%T.D.

Claims (1)

1. thorium uranium mixed oxide ceramic microsphere preparation method, comprise colloidal sol preparation, dispersion gelling, washing, drying and calcining and reduction and sinter each technique, concrete steps are as follows:
Step one colloidal sol preparing process: thorium nitrate is joined in acid deficient uranyl nitrate solution and dissolve, the wherein NO of acid deficient uranyl nitrate solution 3 -/ U (mol ratio)=1.5 ~ 1.8; Th/ (Th+U) (mol ratio)=0.1 ~ 0.5; It is 2.31mol/L that gained mixed solution adds the concentration sum that deionized water is adjusted to uranium and thorium, then this mixed solution is cooled to 0 DEG C ~ 5 DEG C, slowly adds urea and urotropine, be mixed with the colloidal sol of homogeneous transparent, wherein the material of urea 'sthe material of amount and uranium and thorium 'sthe ratio of amount sum is 1.3 ~ 1.8, the material of urotropine 'sthe material of amount and uranium and thorium 'sthe ratio of amount sum is 1.3 ~ 2.2;
Step 2 dispersion gelatinizing process: be distributed in the gelation media 2-Ethylhexyl Alcohol of 60 DEG C ~ 95 DEG C by diverting device by colloidal sol, gelling becomes gel ball;
Step 3 washing process: the mixed solution of gel ball ammoniacal liquor and ethanol is washed, NH in cleansing solution 4oH concentration is 0.5 ~ 3.0mol/L, C 2h 5the percent by volume of OH is 50%, and washing times is 3 ~ 4 times, at every turnwash time is 20 ~ 50min;
Step 4 drying and calcining process: the gel ball after washing is placed in drying calciner drying and calcining, makes it to change into ThO 2-UO 3microballoon, adds the humidity of water management drying and calcining process, and wherein amount of water is 1000 ml ~ 2000ml, and heating schedule is: rise to 80 DEG C at 90min ~ 120min from room temperature, then rises to 90 DEG C at 60min ~ 80min; Then in 90min ~ 120min, 150 DEG C are risen to, insulation 90min ~ 180min; 200 DEG C are risen to subsequently, insulation 50min ~ 80min at 50min ~ 80min; 350 DEG C are risen to again, insulation 60min ~ 150min at 50min ~ 80min;
Step 5 reduction sintering process: by the ThO after drying and calcining 2 -UO 3 microballoon is carry out reduction sintering under the hydrogen atmosphere of 1200 DEG C ~ 1500 DEG C in sintering temperature,obtain the fine and close ThO that diameter is 0.05 ~ 0.2mm 2-UO 2ceramic microsphere.
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CN103366846B (en) * 2013-07-19 2015-08-12 清华大学 Uranium dioxide core ageing tank, ageing, washing drying system and method
CN104671797B (en) * 2015-02-09 2017-02-22 清华大学 Internal gelation method for ceramic microspheres capable of keeping gel solution steady at normal temperature
CN106145198A (en) * 2016-06-29 2016-11-23 中国科学技术大学 Prepare the method and device of uranium oxide microsphere
CN106128516B (en) * 2016-07-15 2017-12-15 中国核动力研究设计院 A kind of thorium base fuel component and small-sized presurized water reactor
CN106297904B (en) * 2016-08-25 2018-04-17 中广核研究院有限公司 UO2The preparation method of SiC fuel pellets and using UO made of the preparation method2SiC fuel pellets
CN106629854B (en) * 2016-10-20 2017-12-15 核工业理化工程研究院 The method of microwave heating uranyl nitrate solution production orange oxide
CN107833645B (en) * 2017-10-26 2020-02-07 中国科学院上海应用物理研究所 Preparation method of thorium-based mixed oxide ceramic microspheres
CN107910084B (en) * 2017-11-21 2020-01-03 中国科学技术大学 Uranium carbide nuclear fuel microsphere and preparation method thereof
CN113753956B (en) * 2021-09-02 2022-11-01 中国原子能科学研究院 Micron-sized monodisperse uranium-thorium mixed particle and preparation method and preparation system thereof

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