CN102496395B - Dispersion column system - Google Patents

Dispersion column system Download PDF

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CN102496395B
CN102496395B CN201110376691.1A CN201110376691A CN102496395B CN 102496395 B CN102496395 B CN 102496395B CN 201110376691 A CN201110376691 A CN 201110376691A CN 102496395 B CN102496395 B CN 102496395B
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ammoniacal liquor
main
ammonia
post
liquor post
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CN102496395A (en
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郝少昌
赵兴宇
马景陶
王阳
邓长生
周湘文
刘兵
唐亚平
梁彤祥
郭文利
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Tsinghua University
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract

The present invention relates to the technical field of sol boiling, and specifically discloses a dispersion column system. The system comprises: a main ammonia water column, an accessory ammonia water column connected with the main ammonia water column, and a storage tank connected with the bottom end of the main ammonia water column through a pipeline, wherein the storage tank is provided with an accessory circulating ammonia water inlet, an accessory circulating ammonia water outlet and a main circulating ammonia water outlet, and the bottom of the accessory ammonia water column is provided with a main circulating ammonia water inlet. With the dispersion column system of the present invention, the stability of the ammonia of the system can be ensured, and the stabilities of the ammonia water liquid level and the ammonia water circulation can be ensured.

Description

Dispersion column system
Technical field
The present invention relates to boil glue technical field, relate in particular to a kind of dispersion column system for the preparation of being applicable to sol-gal process and preparing colloidal sol in ceramic microsphere technique.
Background technology
Sol-gal process is prepared the uranium dioxide core core that ceramic microsphere technique is applied to prepare high temperature gas cooled reactor spheric fuel element conventionally, requires that this uranium dioxide fuel core core density is high, intensity is large and ball-type degree is good.Adopting sol-gal process to prepare uranium dioxide core core mainly comprises the following steps:
1, dissolve: by triuranium octoxide (U 3o 8) powder dissolution in nitric acid, be configured to the uranyl nitrate solution of certain uranium atom concentration;
2, boil glue: in uranyl nitrate solution, by certain metering ratio, add urea, evaporation and concentration certain hour is to certain volume at a certain temperature, add thickening agent to adjust viscosity after cooling, obtain colloidal sol glue;
3, disperse granulation: the glue of getting ready is moved in head tank, with certain pressure, promote glue along Flows, glue is finally admitted to the vibrating nozzle with certain frequency vibration, from flowing out, vibrating nozzle disperses to become the drop with certain size, this step needs the accurate flow of controlling, because the difference of flow directly causes the deviation of drop size;
4, gelling balling-up: drop forms afterwards first through air zone, rely on the surface tension of self to form spherical, spherical droplets is again by ammonia district, spherical droplets and ammonia generation gelling reaction make surperficial precuring and have certain intensity, enter afterwards ammoniacal liquor district and carry out further gelling reaction and become gel ball;
5, ageing: when gel ball has just formed, gelling reaction only completes at gel ball near surface, gel ball internal-response needs regular hour and temperature, therefore gel ball need to be placed in to ammoniacal liquor adds thermal aging 1~3 hour, gel ball is reacted completely, become the spheric grain that has uniformly some strength;
6, washing: uranyl nitrtate reacts with ammoniacal liquor and generates ammonium diuranate and ammonium nitrate, ammonium diuranate is required composition, and ammonium nitrate is objectionable constituent, easily in subsequent technique, causes little ball fractured, therefore ammonium nitrate must be removed, the method conventionally adopting is cyclic washing.Washing needs 3~5 times, and first pass is used 1%~2% weak aqua ammonia, and follow-up several all over using deionized water, each washing lotion need to be tested its concentration of nitric acid, guarantees that nitrate radical content is enough low;
7, dry: the bead after washing is dry by vacuum rotating seasoning, need to control temperature, vacuum tightness and rotational speed, to guarantee that dry run fully completes and can not cause the destruction of bead;
8, roasting: dried bead need to be at roasting kiln roasting, and to slough the organic components in bead, the principal ingredient of the bead after roasting simultaneously becomes orange oxide;
9, reduction: roasting ball, in reduction furnace, is reduced to uranium dioxide under hydrogen atmosphere, need to guarantee the reductive agent of suitable reduction temperature, abundance and the recovery time of abundance;
10, sintering: the bead after reduction, under hydrogen atmosphere, 1400~1600 degrees Celsius of lower sintering 3~5 hours, becomes uranium dioxide core core;
11, screening and sorting: through screening and sorting step, can obtain size homogeneous, the uranium dioxide core core that sphericity meets the demands.
In the above-mentioned process of preparing uranium dioxide core core, it is the committed step of sol-gal process that step 3 is disperseed granulation, first this step is dispersed into uniform droplet by vibrating nozzle by glue, it is spherical that droplet relies on the surface tension of self to form in air, spherical droplets is again by ammonia district, drop and ammonia generation gelling reaction make surperficial precuring and have certain intensity, enter afterwards ammoniacal liquor district and carry out further gelling reaction and become gel ball.This step directly has influence on ball-type degree and the physical property of final products, and the dispersion granulation process of therefore controlling well is most important to whole technique.Disperseing the visual plant of granulation is exactly dispersion column system, and dispersion column system completes the surface cure of particle to the significant process of inner homogenization, therefore optimizes dispersion column system significant.
There are some key issues in existing dispersion column system, for example formation in ammonia district and stable problem, and the stable problem of ammoniacal liquor liquid level, prevents ammonia overflow problem, the motion problems of particle in whole system etc.The stable problem of ammoniacal liquor liquid level has influence on the stability in ammonia district, because the unstable meeting of ammonia circulation of ammonia district causes two kinds of consequences, and the one, the curing deficiency of particle surface causes entering ammoniacal liquor and is hit and flattens, and another kind is the distortion that drop causes due to gravity; Particle is temporary in hold-up vessel, and just curing granule strength is very little, easily in accumulation deposit process, flattens.
Summary of the invention
(1) technical matters that will solve
The technical problem to be solved in the present invention is how to guarantee that the ammonia of dispersion column system is stable, guarantees the stable of ammoniacal liquor liquid level and ammonia circulation.
(2) technical scheme
In order to solve the problems of the technologies described above, the invention provides a kind of dispersion column system, comprising:
Main ammoniacal liquor post, the secondary ammoniacal liquor post being connected with described main ammoniacal liquor post, the hold-up vessel being connected by pipeline with the bottom of described main ammoniacal liquor post, on described hold-up vessel, there is secondary cyclic ammonia water entrance, the outlet of secondary cyclic ammonia water and the outlet of major cycle ammoniacal liquor, described secondary ammoniacal liquor column bottom has major cycle ammonia inlet, secondary ammoniacal liquor post and main ammoniacal liquor post are set up in parallel, its bottom and main ammoniacal liquor post are in same level, its top is higher than the top of main ammoniacal liquor post, secondary ammoniacal liquor post is for the circulation of ammoniacal liquor, and secondary ammoniacal liquor post is connected by connecting pipe with main ammoniacal liquor post.
Further, the top of described main ammoniacal liquor post is connected with run-down pipe, and described run-down pipe is connected with hold-up vessel.
Further, the top of described main ammoniacal liquor post is equipped with ammonia cover, and the top of described ammonia cover connects device for absorbing tail gas.
Further, on described main ammoniacal liquor post and the tank connected pipeline of storage, have particle outlet, described particle outlet bottom has operation valve.
Further, in described hold-up vessel, be provided with filter.
Further, described secondary cyclic ammonia water entrance is positioned at the below of filter, and described secondary cyclic ammonia water outlet is positioned at the top of filter.
Further, the bottom of described hold-up vessel is provided with discharge valve and discharge port.
Further, described main ammoniacal liquor post is connected by connecting pipe with secondary ammoniacal liquor post.
Further, described major cycle ammonia inlet is connected with pump.
Further, described main ammoniacal liquor post is made by transparent material, and described hold-up vessel is hydrostatic column, has conical lower portion.
(3) beneficial effect
Technique scheme has following beneficial effect:
1, the present invention realizes the stable supply of ammoniacal liquor by the main ammonia circulation system consisting of the outlet of major cycle ammoniacal liquor, major cycle ammonia inlet, hold-up vessel, magnetic drive pump, main ammoniacal liquor post, secondary ammoniacal liquor post, connecting pipe and run-down pipe, and wherein main ammoniacal liquor post relies on secondary ammoniacal liquor post and connecting pipe to obtain continuous ammoniacal liquor supply;
2, main ammoniacal liquor post of the present invention keeps the stable of liquid level by ammonia cover and run-down pipe, in main ammoniacal liquor post, by other external units, provide continuous ammonia to supply, keep the stable of ammonia concn, Ye Wei ammonia district provides sufficient ammonia, and these designs have met stable ammonia and ammoniacal liquor supply;
3, the present invention prevents that by being positioned at the device for absorbing tail gas of ammonia cover upper end ammonia overflow from can effectively prevent that ammonia from stop up vibrating nozzle;
4, the present invention makes the particle in hold-up vessel rotatablely move with ammoniacal liquor by the secondary ammonia circulation system being comprised of secondary ammonia circulation outlet, secondary ammonia circulation entrance and magnetic drive pump, has avoided piling up the distortion that extruding causes;
5, the present invention has been avoided fluid and has been stored tank skin peening particle by tangential liquid inflow mode;
6, the present invention prevents that by increasing filter two ammonia circulation systems from bringing particle to damage into.
Accompanying drawing explanation
Fig. 1 is the structural representation of the dispersion column system of the embodiment of the present invention.
Wherein, 1: main ammoniacal liquor post; 2: secondary ammoniacal liquor post; 3: connecting pipe; 4: ammonia cover; 5: run-down pipe; 6: particle outlet; 7: hold-up vessel; 8: filter; 9: discharge valve; 10: secondary cyclic ammonia water outlet; 11: secondary cyclic ammonia water entrance; 12: the outlet of major cycle ammoniacal liquor; 13: major cycle ammonia inlet.
Embodiment
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is described in further detail.Following examples are used for illustrating the present invention, but are not used for limiting the scope of the invention.
As shown in Figure 1, be the structural representation of the dispersion column system of the embodiment of the present invention, this dispersion column system comprises:
Main ammoniacal liquor post 1, the key reaction region for granulation, is made by transparent material, to observe at any time granulation situation.
Secondary ammoniacal liquor post 2 is set up in parallel with main ammoniacal liquor post 1, and its bottom and main ammoniacal liquor post 1 are in same level, and its top is higher than the top of main ammoniacal liquor post 1, and secondary ammoniacal liquor post 2 is for the circulation of ammoniacal liquor, and secondary ammoniacal liquor post 2 is connected by connecting pipe 3 with main ammoniacal liquor post 1;
Hold-up vessel 7, is hydrostatic column, has conical bottom; By pipeline, be connected with main ammoniacal liquor post 1, for storage granules and cyclic ammonia water is provided, in hold-up vessel 7, be provided with filter 8, for intercepting particle, prevent that particle is brought in cyclic ammonia water and is destroyed; In the conical bottom of hold-up vessel 7, be provided with discharge valve 9 and discharge port, this discharge valve 9 is ball valve, for hold-up vessel 7 is endocorpuscular, draws off;
On hold-up vessel 7, be provided with secondary cyclic ammonia water entrance 11 and secondary cyclic ammonia water outlet 10, be respectively the entrance and exit of the circulation stirring ammoniacal liquor in hold-up vessel 7; Wherein secondary cyclic ammonia water entrance 11 is positioned at the below of filter 8, and secondary cyclic ammonia water outlet 10 is positioned at filter 8 tops; Liquid inflow direction is horizontal direction along the tangential direction of hold-up vessel 7 outer walls;
On hold-up vessel 7, being also provided with major cycle ammoniacal liquor outlet 12, is the outlet of whole system cyclic ammonia water, and the bottom of secondary ammoniacal liquor post 2 has major cycle ammonia inlet 13, is positioned at filter 8 tops, is the entrance of whole system cyclic ammonia water; Major cycle ammonia inlet 13 is connected with pump, and liquid stream is by the secondary ammoniacal liquor post 2 of pump Driver injection, and the pump in the present embodiment can be magnetic drive pump.
The top of main ammoniacal liquor post 1 is connected with run-down pipe 5, and is provided with ammonia cover 4, and run-down pipe 5 is connected with hold-up vessel 7, for the part cyclic ammonia water overflowing from main ammoniacal liquor post 1 is guided to hold-up vessel 7, is conducive to keep upper liquid level stable of main ammoniacal liquor post 1; Ammonia cover 4 is assemblied in the top of main ammoniacal liquor post 1, forms a cavity above main ammoniacal liquor post 1, forms ammonia district; Ammonia cover 4 tops are offered porose and are connected with device for absorbing tail gas, for absorbing unnecessary ammonia, prevent that ammonia is from the 4 top effect of flood granulations of ammonia cover;
The bottom of main ammoniacal liquor post 1 is also provided with particle outlet 6, and for the discharge of main ammoniacal liquor post 1 internal particle and the circulation of ammoniacal liquor, the particle that is discharged to hold-up vessel 7 is intercepted by filter 8, can further not be recycled in main ammoniacal liquor post 1 and secondary ammoniacal liquor post 2.
The bottom of particle outlet 6 is provided with operation valve, is specially control ball valve, for controlling main ammoniacal liquor post 1, discharges the speed of ammoniacal liquor toward hold-up vessel 7.
As can be seen from the above embodiments, the dispersion column system that the embodiment of the present invention provides has following beneficial effect:
1, the present invention realizes the stable supply of ammoniacal liquor by the main ammonia circulation system consisting of the outlet of major cycle ammoniacal liquor, major cycle ammonia inlet, hold-up vessel, magnetic drive pump, main ammoniacal liquor post, secondary ammoniacal liquor post, connecting pipe and run-down pipe, and wherein main ammoniacal liquor post relies on secondary ammoniacal liquor post and connecting pipe to obtain continuous ammoniacal liquor supply;
2, main ammoniacal liquor post of the present invention keeps the stable of liquid level by ammonia cover and run-down pipe, in main ammoniacal liquor post, by other external units, provide continuous ammonia to supply, keep the stable of ammonia concn, Ye Wei ammonia district provides sufficient ammonia, and these designs have met stable ammonia and ammoniacal liquor supply;
3, the present invention prevents that by being positioned at the device for absorbing tail gas of ammonia cover upper end ammonia overflow from can effectively prevent that ammonia from stop up vibrating nozzle;
4, the present invention makes the particle in hold-up vessel rotatablely move with ammoniacal liquor by the secondary ammonia circulation system being comprised of secondary ammonia circulation outlet, secondary ammonia circulation entrance and magnetic drive pump, has avoided piling up the distortion that extruding causes;
5, the present invention has been avoided fluid and has been stored tank skin peening particle by tangential liquid inflow mode;
6, the present invention prevents that by increasing filter two ammonia circulation systems from bringing particle to damage into.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, do not departing under the prerequisite of the technology of the present invention principle; can also make some improvement and modification, these improve and modification also should be considered as protection scope of the present invention.

Claims (9)

1. a dispersion column system, is characterized in that, comprising:
Main ammoniacal liquor post, the secondary ammoniacal liquor post being connected with described main ammoniacal liquor post, the hold-up vessel being connected by pipeline with the bottom of described main ammoniacal liquor post, on described hold-up vessel, there is secondary cyclic ammonia water entrance, the outlet of secondary cyclic ammonia water and the outlet of major cycle ammoniacal liquor, described secondary ammoniacal liquor column bottom has major cycle ammonia inlet, secondary ammoniacal liquor post and main ammoniacal liquor post are set up in parallel, its bottom and main ammoniacal liquor post are in same level, its top is higher than the top of main ammoniacal liquor post, secondary ammoniacal liquor post is for the circulation of ammoniacal liquor, and secondary ammoniacal liquor post is connected by connecting pipe with main ammoniacal liquor post.
2. dispersion column system as claimed in claim 1, is characterized in that, the top of described main ammoniacal liquor post is connected with run-down pipe, and described run-down pipe is connected with hold-up vessel.
3. dispersion column system as claimed in claim 1, is characterized in that, the top of described main ammoniacal liquor post is equipped with ammonia cover, and the top of described ammonia cover connects device for absorbing tail gas.
4. dispersion column system as claimed in claim 1, is characterized in that, on described main ammoniacal liquor post and the tank connected pipeline of storage, has particle outlet, and described particle outlet bottom has operation valve.
5. dispersion column system as claimed in claim 1, is characterized in that, in described hold-up vessel, is provided with filter.
6. dispersion column system as claimed in claim 5, is characterized in that, described secondary cyclic ammonia water entrance is positioned at the below of filter, and described secondary cyclic ammonia water outlet is positioned at the top of filter.
7. dispersion column system as claimed in claim 5, is characterized in that, the bottom of described hold-up vessel is provided with discharge valve and discharge port.
8. dispersion column system as claimed in claim 1, is characterized in that, described major cycle ammonia inlet is connected with pump.
9. dispersion column system as claimed in claim 1, is characterized in that, described main ammoniacal liquor post is made by transparent material, and described hold-up vessel is hydrostatic column, has conical lower portion.
CN201110376691.1A 2011-11-23 2011-11-23 Dispersion column system Active CN102496395B (en)

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Publication number Priority date Publication date Assignee Title
CN102838167A (en) * 2012-09-11 2012-12-26 清华大学 Dispersion column system
CN103310858B (en) * 2013-06-28 2015-12-02 清华大学 A kind of pellet charge device and method
CN104526837B (en) * 2014-12-23 2017-06-06 清华大学 The equipment for preparing ceramic microsphere
CN108777179B (en) * 2018-06-13 2020-03-27 清华大学 Gel ball normal temperature aging device

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006062886A (en) * 2004-08-24 2006-03-09 Nuclear Fuel Ind Ltd Method and apparatus for producing ammonium diuranate particle
CN1935478A (en) * 2006-10-16 2007-03-28 清华大学 Method and apparatus for preparing ceramic microball by injection-condensation
CN1937097A (en) * 2006-10-16 2007-03-28 清华大学 Technology for making nuclear fuel element core by external gelatinization method
CN101912747A (en) * 2009-11-12 2010-12-15 天津大学 Vibration crushing type granulation system and method of metal oxide particle

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US20080152393A1 (en) * 2006-12-20 2008-06-26 Masashi Nagayama Carrier for electrophotographic developer, image forming method, and process cartridge

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006062886A (en) * 2004-08-24 2006-03-09 Nuclear Fuel Ind Ltd Method and apparatus for producing ammonium diuranate particle
CN1935478A (en) * 2006-10-16 2007-03-28 清华大学 Method and apparatus for preparing ceramic microball by injection-condensation
CN1937097A (en) * 2006-10-16 2007-03-28 清华大学 Technology for making nuclear fuel element core by external gelatinization method
CN101912747A (en) * 2009-11-12 2010-12-15 天津大学 Vibration crushing type granulation system and method of metal oxide particle

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