CN104446479A - Method of preparing ceramic grade uranium dioxide ball - Google Patents

Method of preparing ceramic grade uranium dioxide ball Download PDF

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Publication number
CN104446479A
CN104446479A CN201410618651.7A CN201410618651A CN104446479A CN 104446479 A CN104446479 A CN 104446479A CN 201410618651 A CN201410618651 A CN 201410618651A CN 104446479 A CN104446479 A CN 104446479A
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ball
ceramic grade
uranium dioxide
green compact
high temperature
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汪新杰
尹荣才
刘锦洪
卢长先
李佳
周劲松
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Nuclear Power Institute of China
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Nuclear Power Institute of China
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Abstract

The invention discloses a method of preparing a ceramic grade uranium dioxide ball. The method sequentially comprises the following steps: carrying out ball milling on uranium oxide, wherein the particle size of the uranium oxide after ball milling is 0.1-0.3 micron; adding the uranium oxide into a polymer monomer, and uniformly stirring to obtain polymer slurry; producing slurry drops by virtue of the polymer slurry; adding the slurry drops into a dispersion column which contains heated carbon tetrachloride or liquid paraffin, and descending the slurry drops to obtain a green body ball in the dispersion column under the surface tension, wherein the temperature in the dispersion column is 80-90 DEG C; washing the green body ball by adopting an ethanol solution; drying the green body ball, and removing an organic matter on the surface of the green body ball to obtain a dry calcined ball; and carrying out reduction sintering on the dry calcined ball in a hydrogen atmosphere to obtain the ceramic grade UO2 ball. The method is simple in whole process, convenient in realization, small in introduced impurities, high in purity of the prepared UO2 ball and beneficial to popularizing and applying the UO2 ball in the field of nuclear technology.

Description

A kind of method preparing ceramic grade uranium dioxide ball
Technical field
The present invention relates to nuclear matter manufacturing process, specifically a kind of method preparing ceramic grade uranium dioxide ball.
Background technology
In nuclear technology field, UO 2napiform root has different purposes according to the difference of size, and wherein, in nuclear technology field, diameter is the UO of 0.5 ~ 3mm 2ball is most widely used, as: diameter is the UO of 0.5mm 2ball can be used as the fuel of high temperature gas cooled reactor, and diameter is the UO of 0.8 ~ 1.0mm 2ball may be used for the development of neutron detector.Now at preparation UO 2during ball, operation sequence is complicated, introduces impurity more, UO 2the purity of ball can not be guaranteed, and this can affect UO 2ball applying at nuclear technology field.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of method preparing ceramic grade uranium dioxide ball, the method simple operation, be convenient to realize, introduce impurity few, the UO of preparation 2ball purity is high, and then is conducive to UO 2ball applying at nuclear technology field.
The present invention solves the problem and is achieved through the following technical solutions:
Prepare a method for ceramic grade uranium dioxide ball, comprise the following steps of carrying out successively:
Step one, by uranium oxide ball milling, wherein, after ball milling, uranium oxide granularity is 0.1 ~ 0.3 μm;
Step 2, uranium oxide is added polymer monomer, and stir and obtain polymer paste;
Step 3, polymer paste is generated slurry drip;
Step 4, slurry is added dropwise to heating tetracol phenixin or liquid paraffin are housed dispersion column in, wherein, in dispersion column, temperature is 80 ~ 90 DEG C, and slurry drops in dispersion column and declines and under surface tension effects, obtain green compact ball in dispersion column;
Step 5, employing ethanolic soln wash green compact ball;
Step 6, by green compact ball, the dry and organism removing surface obtains dryly forging ball;
Step 7, by dry forge ball under an atmosphere of hydrogen through reduction sintering obtain ceramic grade UO 2ball.
Further, the uranium oxide adopted in described step one is U 3o 8powder, UO 2powder or U 3o 8powder and UO 2the mixture of powder.
Further, the ammonium citrate adding uranium oxide consumption 0.1wt % ~ 3wt% or ammonium polyacrylate is also comprised in described step 2.Wherein, ammonium citrate or ammonium polyacrylate are as dispersion agent, ammonium citrate or ammonium polyacrylate are all a kind of interfacial agents simultaneously in molecule with lipophilicity and wetting ability two kinds of opposite nature, can homogeneous dispersion those be difficult to be dissolved in the inorganic of liquid, the solid particulate of pigment dyestuff, also can prevent sedimentation and the cohesion of solid particulate simultaneously.
Further, involved in described step 2 to step 4 pipeline and device temperature be not all higher than 10 DEG C.Monomer polymerization speed of the present invention is very fast, to sharply increase once polymeric size viscosity, the final dispersion affecting slurry, therefore, the present invention is by reducing temperature, effectively can reduce the speed of reaction of course of conveying, guarantee the stability of slurry in preparation and course of conveying, ensure that technique is carried out smoothly.
Further, in described step 5, the volume by volume concentration of ethanolic soln is 70% ~ 90%, and the consumption of described ethanolic soln and the volume ratio of green compact ball are 1:1 ~ 4:1.
Further, in described step 6, the drying of green compact ball is carried out in high temperature oven, and in high temperature oven, initial temperature is 25 DEG C, and drying process is carried out according to the following steps successively:
Temperature in high temperature oven is risen to 80 DEG C by 25 DEG C by steps A, 90 minutes used times gradually;
Temperature in high temperature oven is risen to 150 DEG C by 80 DEG C by step B, 120 minutes used times gradually;
Temperature in high temperature oven is risen to 200 DEG C by 150 DEG C by step C, 120 minutes used times gradually;
Temperature in high temperature oven is risen to 400 DEG C by 200 DEG C by step D, 150 minutes used times gradually;
Step e, by greenhouse cooling in high temperature oven to room temperature.When the present invention applies, adopt and to heat up gradually drying, wherein, 25 DEG C are warming up to 90 minutes 80 DEG C of used times, and 80 DEG C are warming up to 120 minutes 150 DEG C of used times, 150 DEG C to being warming up to 120 minutes 200 DEG C of used times, 200 DEG C are warming up to 150 minutes 400 DEG C of used times.The compositions such as polymeric skeleton, inorganic salt, water need be removed when the present invention applies, wherein, the removal temperature of different compositions is different, removal temperature as water is 80 DEG C ~ 120 DEG C, the removal temperature of inorganic salt is 180 DEG C ~ 220 DEG C, the removal temperature of polymeric skeleton is 350 DEG C ~ 400 DEG C, water or inorganic salt will be made to remove rapidly if be directly warming up to 400 DEG C, easily causes the green compact ball cracking manufactured.Therefore, the present invention adopts the mode of temperature programming, can remove in interval fully to complete in the temperature of different components to remove, and ensure that ceramic grade UO 2the qualification rate of ball.
As the first embodiment of the polymer monomer that the present invention adopts, the polymer monomer added in described step 2 comprises urea and urotropine, wherein, in polymer paste, uranium oxide content is 30wt% ~ 50wt%, urea content is 120 ~ 180g/L, and urotropine content is 300 ~ 450g/L.
As the second embodiment of the polymer monomer that the present invention adopts, the polymer monomer added in described step 2 comprises acrylamide and N, N-methylene-bisacrylamide, wherein, in polymer paste, uranium oxide content is 40wt% ~ 60wt%, acrylamide content is 10wt % ~ 20wt%, and N,N methylene bis acrylamide is 1wt % ~ 2wt%.
Further, the ammonium persulphate adding polymer monomer consumption 0.1wt % ~ 1wt % is also comprised in described step 2.Wherein, ammonium persulphate is as initiator, and it is for acrylamide triggered and radical polymerization that is N,N methylene bis acrylamide.
The volume further, being also included in dispersion column and adding N, N, N, N in described step 4 the consumption of '-Tetramethyl Ethylene Diamine, N, N, N, N '-Tetramethyl Ethylene Diamine is 0.05% ~ 0.1% of tetracol phenixin or liquid paraffin volume.Wherein, N, N, N, N '-Tetramethyl Ethylene Diamine as catalyzer for the preparation of the larger UO of diameter 2add during ball.
In sum, the present invention has following beneficial effect: simple operation when (1) the present invention applies, and is convenient to realize, and is convenient to obtain uranium oxide green compact ball, without the need to mould, introduces impurity few in the present invention, the UO of preparation 2ball purity is high, and then is conducive to UO 2ball applying at nuclear technology field.
(2) the present invention only need remove tetrachloro and enters carbon or whiteruss when cleaning green compact ball, and cleaning is convenient, is convenient to realize.
Embodiment
Below in conjunction with embodiment, detailed description is further done to the present invention, but embodiments of the present invention are not limited thereto.
Embodiment 1:
Prepare a method for ceramic grade uranium dioxide ball, comprise the following five steps carried out successively: slurry preparation, dispersion gelling, washing, drying and calcining and reduction sintering.The detailed process of slurry preparation is: by U 3o 8powder weighing 50.4g adds water for ball milling 2h and obtains U 3o 8slurry, U in ball milling disposed slurry 3o 8powder mean sizes is 0.2 μm.By U 3o 8slurry is placed in 10 DEG C of isoperibols, treats that temperature is reduced to less than 10 DEG C and adds 12 grams, urea, urotropine 28 grams, ammonium citrate 1.1g, and stirs and obtain polymer paste.
The detailed process of dispersion gelling is: added by polymer paste in vibration dispersion device, vibration dispersion device has the uniform orifice plate in three holes, the slurry that Vibration on Start-up diverting device makes polymer paste obtain certain size by the through hole on orifice plate when dispersive pressure in it is 0.15MPa drips, and slurry drips through carrier band transmission and falls into the CCl that heating is housed 4dispersion column in, balling-up under surface tension effects in dispersion column, and in decline process polymerization obtain green compact ball.Wherein, dispersion column length 2.5m, in dispersion column, medium temperature should maintain 85 DEG C, and the present embodiment controls the diameter of green compact ball by the vibrational frequency of flow and vibration dispersion device, and the pipeline of dispersion involved by gelling and device temperature be not all higher than 10 DEG C.
Washing detailed process be: adopt volume by volume concentration be 70% ethanolic soln green compact ball is cleaned, the consumption of ethanolic soln and the volume ratio of green compact ball are 3:1, and scavenging period is 1h.The detailed process of drying and calcining is: green compact ball is put into high temperature oven and heat up gradually and carry out drying and calcining, and green compact ball completes dehydration and removes organism and obtains dryly forging ball in the process of drying and calcining.Wherein, in high temperature oven, the concrete process heated up is: 90 minutes used times were warming up to 80 DEG C gradually by 25 DEG C, 120 minutes used times were warming up to 150 DEG C gradually by 80 DEG C, 120 minutes used times were warming up to 200 DEG C gradually by 150 DEG C, 150 minutes used times were warming up to 400 DEG C gradually by 200 DEG C, were then cooled to 25 DEG C.The detailed process of reduction sintering is: dry ball of forging is obtained ceramic grade UO through reduction sintering under an atmosphere of hydrogen 2ball.
Adopt the ceramic grade UO that the present embodiment prepares 2the diameter of ball is 1.0 ~ 1.2mm, O/U is 1.99, and sphericity is less than 1.07.
Embodiment 2:
Prepare a method for ceramic grade uranium dioxide ball, comprise the following five steps carried out successively: slurry preparation, dispersion gelling, washing, drying and calcining and reduction sintering.The detailed process of slurry preparation is: by U 3o 8powder weighs 33.6g ball milling 3h and obtains U 3o 8powder, U after ball milling 3o 8powder mean sizes is 0.18 μm.In 10 DEG C of isoperibols, by water/acrylamide/N,N methylene bis acrylamide according to the proportions pre-polymerization liquid of 100/15/1, add U 3o 8powder also stirs and obtains polymer paste, adds the ammonium persulphate of acrylamide and N,N methylene bis acrylamide gross weight 1%, and adds U 3o 8the ammonium citrate of powder weight 2%, wherein, U 3o 8content in polymer paste is 45wt%.
The detailed process of dispersion gelling is: added by polymer paste in vibration dispersion device, vibration dispersion device has the uniform orifice plate in four holes, the slurry that Vibration on Start-up diverting device makes polymer paste obtain certain size by the through hole on orifice plate when dispersive pressure in it is 0.15MPa drips, slurry drips through carrier band transmission and falls in the dispersion column of the paraffin that heating is housed, balling-up under surface tension effects in dispersion column, and polymerization obtains green compact ball in decline process.Wherein, dispersion column length 3m, in dispersion column, medium temperature should maintain 85 DEG C, and the present embodiment controls the diameter of green compact ball by the vibrational frequency of flow and vibration dispersion device, and the pipeline of dispersion involved by gelling and device temperature be not all higher than 10 DEG C.
Washing detailed process be: adopt volume by volume concentration be 80% ethanolic soln green compact ball is cleaned, the consumption of ethanolic soln and the volume ratio of green compact ball are 4:1, and scavenging period is 0.5h.The detailed process of drying and calcining is: green compact ball is put into high temperature oven and heat up gradually and carry out drying and calcining, and green compact ball completes dehydration and removes organism and obtains dryly forging ball in the process of drying and calcining.Wherein, in high temperature oven, the concrete process heated up is: 90 minutes used times were warming up to 80 DEG C gradually by 25 DEG C, 120 minutes used times were warming up to 150 DEG C gradually by 80 DEG C, 120 minutes used times were warming up to 200 DEG C gradually by 150 DEG C, 150 minutes used times were warming up to 400 DEG C gradually by 200 DEG C, were then cooled to 25 DEG C.The detailed process of reduction sintering is: dry ball of forging is obtained ceramic grade UO through reduction sintering under an atmosphere of hydrogen 2ball.
Adopt the ceramic grade UO that the present embodiment prepares 2the diameter of ball is 0.5 ~ 0.6mm, O/U is 1.99, and sphericity is less than 1.05.
Embodiment 3:
Prepare a method for ceramic grade uranium dioxide ball, comprise the following five steps carried out successively: slurry preparation, dispersion gelling, washing, drying and calcining and reduction sintering.The detailed process of slurry preparation is: by U 3o 8powder weighs 54.0g ball milling 8h and obtains U 3o 8powder, U after ball milling 3o 8powder mean sizes is 0.27 μm.In 10 DEG C of isoperibols, by water/acrylamide/N,N methylene bis acrylamide according to the proportions pre-polymerization liquid of 100/20/1.5, add U 3o 8powder also stirs and obtains polymer paste, adds the ammonium persulphate of acrylamide and N,N methylene bis acrylamide gross weight 0.8%, and adds U 3o 8the ammonium polyacrylate of powder weight 2.5%, wherein, U 3o 8content in polymer paste is 55wt%.
Dispersion gelling detailed process be: polymer paste is put into syringe, slowly by pulp jets in the dispersion column of liquid paraffin that heating is housed, balling-up under surface tension effects in dispersion column, and in decline process polymerization obtain green compact ball.Wherein, the N of whiteruss volume 0.05% is added in dispersion column, N, N, N '-Tetramethyl Ethylene Diamine as catalyzer, dispersion column length 3m, in dispersion column, medium temperature should maintain 85 DEG C, the present embodiment is by the diameter of the pressure-controlling green compact ball of syringe, and the pipeline of dispersion involved by gelling and device temperature be not all higher than 10 DEG C.
Washing detailed process be: adopt volume by volume concentration be 85% ethanolic soln green compact ball is cleaned, the consumption of ethanolic soln and the volume ratio of green compact ball are 2:1, and scavenging period is 0.5h.The detailed process of drying and calcining is: green compact ball is put into high temperature oven and heat up gradually and carry out drying and calcining, and green compact ball completes dehydration and removes organism and obtains dryly forging ball in the process of drying and calcining.Wherein, in high temperature oven, the concrete process heated up is: 90 minutes used times were warming up to 80 DEG C gradually by 25 DEG C, 120 minutes used times were warming up to 150 DEG C gradually by 80 DEG C, 120 minutes used times were warming up to 200 DEG C gradually by 150 DEG C, 150 minutes used times were warming up to 400 DEG C gradually by 200 DEG C, were then cooled to 25 DEG C.The detailed process of reduction sintering is: dry ball of forging is obtained ceramic grade UO through reduction sintering under an atmosphere of hydrogen 2ball.
Adopt the ceramic grade UO that the present embodiment prepares 2the diameter of ball is 2.5 ~ 3.0mm, O/U is 2.01, and sphericity is less than 1.1.
Embodiment 4:
Prepare a method for ceramic grade uranium dioxide ball, comprise the following five steps carried out successively: slurry preparation, dispersion gelling, washing, drying and calcining and reduction sintering.The detailed process of slurry preparation is: by 42.0g U 3o 8powder and 13.5gUO 2powder ball milling 3h, after ball milling, powder mean sizes is 0.22 μm.In 10 DEG C of isoperibols, by water/acrylamide/N, N-methylene-bisacrylamide according to 100/10/1.5 proportions pre-polymerization liquid, add the uranium oxide powder after ball milling and stir and obtain polymer paste, add acrylamide and N, the ammonium persulphate of both N-methylene-bisacrylamides gross weight 0.1%, and add U 3o 8the ammonium polyacrylate of powder weight 3%, wherein, the content of uranium oxide in polymer paste is 57wt%.
Dispersion gelling detailed process be: polymer paste is put into syringe, slowly by pulp jets in the dispersion column of liquid paraffin that heating is housed, balling-up under surface tension effects in dispersion column, and in decline process polymerization obtain green compact ball.Wherein, the N of whiteruss volume 0.1% is added in dispersion column, N, N, N '-Tetramethyl Ethylene Diamine as catalyzer, dispersion column length 3m, in dispersion column, medium temperature should maintain 85 DEG C, the present embodiment is by the diameter of the pressure-controlling green compact ball of syringe, and the pipeline of dispersion involved by gelling and device temperature be not all higher than 10 DEG C.
Washing detailed process be: adopt volume by volume concentration be 90% ethanolic soln green compact ball is cleaned, the consumption of ethanolic soln and the volume ratio of green compact ball are 1.5:1, and scavenging period is 0.25h.The detailed process of drying and calcining is: green compact ball is put into high temperature oven and heat up gradually and carry out drying and calcining, and green compact ball completes dehydration and removes organism and obtains dryly forging ball in the process of drying and calcining.Wherein, in high temperature oven, the concrete process heated up is: 90 minutes used times were warming up to 80 DEG C gradually by 25 DEG C, 120 minutes used times were warming up to 150 DEG C gradually by 80 DEG C, 120 minutes used times were warming up to 200 DEG C gradually by 150 DEG C, 150 minutes used times were warming up to 400 DEG C gradually by 200 DEG C, were then cooled to 25 DEG C.The detailed process of reduction sintering is: dry ball of forging is obtained ceramic grade UO through reduction sintering under an atmosphere of hydrogen 2ball.
Adopt the ceramic grade UO that the present embodiment prepares 2the diameter of ball is 1.8 ~ 2.2mm, O/U is 1.99, and sphericity is less than 1.1.
Embodiment 5:
Prepare a method for ceramic grade uranium dioxide ball, comprise the following five steps carried out successively: slurry preparation, dispersion gelling, washing, drying and calcining and reduction sintering.The detailed process of slurry preparation is: by 84.0g U 3o 8powder ball milling 5h, after ball milling, powder mean sizes is 0.19 μm.In 10 DEG C of isoperibols, by water/acrylamide/N, N-methylene-bisacrylamide according to 100/10/1.5 proportions pre-polymerization liquid, add the uranium oxide powder after ball milling and stir and obtain polymer paste, add acrylamide and N, the ammonium persulphate of both N-methylene-bisacrylamides gross weight 0.5%, and add U 3o 8the ammonium polyacrylate of powder weight 2.8%, wherein, the content of uranium oxide in polymer paste is 54wt%.
Dispersion gelling detailed process be: polymer paste is put into syringe, slowly by pulp jets in the dispersion column of liquid paraffin that heating is housed, balling-up under surface tension effects in dispersion column, and in decline process polymerization obtain green compact ball.Wherein, the N of whiteruss volume 0.08% is added in dispersion column, N, N, N '-Tetramethyl Ethylene Diamine as catalyzer, dispersion column length 3m, in dispersion column, medium temperature should maintain 85 DEG C, the present embodiment is by the diameter of the pressure-controlling green compact ball of syringe, and the pipeline of dispersion involved by gelling and device temperature be not all higher than 10 DEG C.
Washing detailed process be: adopt volume by volume concentration be 90% ethanolic soln green compact ball is cleaned, the consumption of ethanolic soln and the volume ratio of green compact ball are 3.8:1, and scavenging period is 0.25h.The detailed process of drying and calcining is: green compact ball is put into high temperature oven and heat up gradually and carry out drying and calcining, and green compact ball completes dehydration and removes organism and obtains dryly forging ball in the process of drying and calcining.Wherein, in high temperature oven, the concrete process heated up is: 90 minutes used times were warming up to 80 DEG C gradually by 25 DEG C, 120 minutes used times were warming up to 150 DEG C gradually by 80 DEG C, 120 minutes used times were warming up to 200 DEG C gradually by 150 DEG C, 150 minutes used times were warming up to 400 DEG C gradually by 200 DEG C, were then cooled to 25 DEG C.The detailed process of reduction sintering is: dry ball of forging is obtained ceramic grade UO through reduction sintering under an atmosphere of hydrogen 2ball.
Adopt the ceramic grade UO that the present embodiment prepares 2the diameter of ball is 2.4 ~ 2.6mm, O/U is 2.01, and sphericity is less than 1.06.
As mentioned above, the present invention can be realized preferably.

Claims (10)

1. prepare a method for ceramic grade uranium dioxide ball, it is characterized in that, comprise the following steps of carrying out successively:
Step one, by uranium oxide ball milling, wherein, after ball milling, uranium oxide granularity is 0.1 ~ 0.3 μm;
Step 2, uranium oxide is added polymer monomer, and stir and obtain polymer paste;
Step 3, polymer paste is generated slurry drip;
Step 4, slurry is added dropwise to heating tetracol phenixin or liquid paraffin are housed dispersion column in, wherein, in dispersion column, temperature is 80 ~ 90 DEG C, and slurry drops in dispersion column and declines and under surface tension effects, obtain green compact ball in dispersion column;
Step 5, employing ethanolic soln wash green compact ball;
Step 6, by green compact ball, the dry and organism removing surface obtains dryly forging ball;
Step 7, by dry forge ball under an atmosphere of hydrogen through reduction sintering obtain ceramic grade UO 2ball.
2. a kind of method preparing ceramic grade uranium dioxide ball according to claim 1, is characterized in that, the uranium oxide adopted in described step one is U 3o 8powder, UO 2powder or U 3o 8powder and UO 2the mixture of powder.
3. a kind of method preparing ceramic grade uranium dioxide ball according to claim 1, is characterized in that, also comprises the ammonium citrate or ammonium polyacrylate that add uranium oxide consumption 0.1wt % ~ 3wt% in described step 2.
4. a kind of method preparing ceramic grade uranium dioxide ball according to claim 1, is characterized in that, pipeline involved in described step 2 to step 4 and device temperature be not all higher than 10 DEG C.
5. a kind of method preparing ceramic grade uranium dioxide ball according to claim 1, is characterized in that, in described step 5, the volume by volume concentration of ethanolic soln is 70% ~ 90%, and the consumption of described ethanolic soln and the volume ratio of green compact ball are 1:1 ~ 4:1.
6. a kind of method preparing ceramic grade uranium dioxide ball according to claim 1, is characterized in that, in described step 6, the drying of green compact ball is carried out in high temperature oven, and in high temperature oven, initial temperature is 25 DEG C, and drying process is carried out according to the following steps successively:
Temperature in high temperature oven is risen to 80 DEG C by 25 DEG C by steps A, 90 minutes used times gradually;
Temperature in high temperature oven is risen to 150 DEG C by 80 DEG C by step B, 120 minutes used times gradually;
Temperature in high temperature oven is risen to 200 DEG C by 150 DEG C by step C, 120 minutes used times gradually;
Temperature in high temperature oven is risen to 400 DEG C by 200 DEG C by step D, 150 minutes used times gradually;
Step e, by greenhouse cooling in high temperature oven to room temperature.
7. according to a kind of method preparing ceramic grade uranium dioxide ball in claim 1 ~ 6 described in any one, it is characterized in that, the polymer monomer added in described step 2 comprises urea and urotropine, wherein, in polymer paste, uranium oxide content is 30wt% ~ 50wt%, urea content is 120 ~ 180g/L, and urotropine content is 300 ~ 450g/L.
8. according to a kind of method preparing ceramic grade uranium dioxide ball in claim 1 ~ 6 described in any one, it is characterized in that, the polymer monomer added in described step 2 comprises acrylamide and N, N-methylene-bisacrylamide, wherein, in polymer paste, uranium oxide content is 40wt% ~ 60wt%, and acrylamide content is 10wt % ~ 20wt%, N,N methylene bis acrylamide is 1wt % ~ 2wt%.
9. a kind of method preparing ceramic grade uranium dioxide ball according to claim 8, is characterized in that, also comprises the ammonium persulphate adding polymer monomer consumption 0.1wt % ~ 1wt % in described step 2.
10. a kind of method preparing ceramic grade uranium dioxide ball according to claim 8, it is characterized in that, also be included in dispersion column in described step 4 and add N, N, N, N '-Tetramethyl Ethylene Diamine, N, N, N, N ' volume of consumption of-Tetramethyl Ethylene Diamine is 0.05% ~ 0.1% of tetracol phenixin or liquid paraffin volume.
CN201410618651.7A 2014-11-06 2014-11-06 Method of preparing ceramic grade uranium dioxide ball Pending CN104446479A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105642907A (en) * 2016-01-29 2016-06-08 中国核动力研究设计院 UO2-W metal ceramic ball preparation method
CN107140953A (en) * 2017-04-18 2017-09-08 华中科技大学 A kind of method that quick extrusion prepares ceramic microsphere
CN107840369A (en) * 2016-09-20 2018-03-27 中核四〇四有限公司 A kind of MOX uranium dioxide preprocessing method of raw materials
CN107837896A (en) * 2016-09-20 2018-03-27 中核四〇四有限公司 A kind of MOX material powders dry ball milling method
CN111032205A (en) * 2017-08-23 2020-04-17 原子能和替代能源委员会 Method for preparing a powder containing uranium oxide UO2, optionally plutonium oxide PuO2, and optionally americium oxide AmO2 and/or other minor actinide oxides
CN111039326A (en) * 2020-01-13 2020-04-21 清华大学 Method for preparing uranium dioxide microspheres at normal temperature

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100999408A (en) * 2006-12-15 2007-07-18 清华大学 Method of preparing UO2 ceramic fuel microsphere

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100999408A (en) * 2006-12-15 2007-07-18 清华大学 Method of preparing UO2 ceramic fuel microsphere

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
顾树川等: "用内胶凝法制备高密度UO2陶瓷微球的实验研究（上）", 《核动力工程》, 30 April 1980 (1980-04-30) *

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105642907A (en) * 2016-01-29 2016-06-08 中国核动力研究设计院 UO2-W metal ceramic ball preparation method
CN107840369A (en) * 2016-09-20 2018-03-27 中核四〇四有限公司 A kind of MOX uranium dioxide preprocessing method of raw materials
CN107837896A (en) * 2016-09-20 2018-03-27 中核四〇四有限公司 A kind of MOX material powders dry ball milling method
CN107140953A (en) * 2017-04-18 2017-09-08 华中科技大学 A kind of method that quick extrusion prepares ceramic microsphere
CN107140953B (en) * 2017-04-18 2019-11-22 华中科技大学 A kind of method that quick extrusion prepares ceramic microsphere
CN111032205A (en) * 2017-08-23 2020-04-17 原子能和替代能源委员会 Method for preparing a powder containing uranium oxide UO2, optionally plutonium oxide PuO2, and optionally americium oxide AmO2 and/or other minor actinide oxides
CN111032205B (en) * 2017-08-23 2022-07-05 原子能和替代能源委员会 Method for preparing a powder containing uranium oxide, optionally plutonium oxide, and optionally americium oxide and/or other minor actinide oxides
CN111039326A (en) * 2020-01-13 2020-04-21 清华大学 Method for preparing uranium dioxide microspheres at normal temperature
CN111039326B (en) * 2020-01-13 2020-12-01 清华大学 Method for preparing uranium dioxide microspheres at normal temperature

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