CN104250002A - Preparation method of crystalline zirconium phosphate for purifying nuclear uranium ions - Google Patents
Preparation method of crystalline zirconium phosphate for purifying nuclear uranium ions Download PDFInfo
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- CN104250002A CN104250002A CN201410524251.XA CN201410524251A CN104250002A CN 104250002 A CN104250002 A CN 104250002A CN 201410524251 A CN201410524251 A CN 201410524251A CN 104250002 A CN104250002 A CN 104250002A
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- zirconium phosphate
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- plastid
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- crystalline zirconium
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Abstract
The invention relates to a preparation method of crystalline zirconium phosphate for purifying nuclear uranium ions. The preparation method comprises the following steps: step 1, uniformly mixing ammonium dihydrogen phosphate and zirconyl chloride octahydrate, which have the same mole number, and roasting the mixture for 1 to 4 hours at the temperature of 1,216 to 1,258 DEG C; step 2, grinding the obtained product into particles with the particle size of about 0.07 to 0.08 mm and after carrying out electromagnetic stirring, performing suction filtration on the particles with deionized water until electrical conductivity of washing water is the same as that of the deionized water; step 3: finally, baking for 2 to 6 hours in a baking oven at the temperature of 80 to 120 DEG C so as to obtain the crystalline zirconium phosphate. According to the invention, by optimizing the roasting temperature and the roasting time, capacity of adsorbing the nuclear uranium ions of the synthesized crystalline zirconium phosphate is further improved and the synthesized crystalline zirconium phosphate is more suitable for treating radioactive chemical nuclear waste.
Description
Technical field
The present invention relates to a kind of preparation method of phosphate material, be specifically related to a kind of preparation method purifying the crystallization plastid zirconium phosphate of core uranium ion.
Background technology
The disposal of crystallization plastid zirconium phosphate to transformation period very long level radioactive nuclear waste core uranium ion is the problem that countries in the world are paid special attention to, for at time of peace as the process of the nuke rubbish of energy utilization and the core radiocontamination for the Nuclear weapons in the wartime, use deep stratum process unanimously to be approved safer treatment process now.Even if but the disposal warehouse of radiation waste material is built at deep stratum, the leakage and polluted underground water that cause level radioactive nuclear waste are held in the activity due to stratum very much, again pollute physical environment.
In order to prevent contaminate environment again, engineering and natural multilayer screen can be used to be isolated by nuke rubbish, the effect of multilayer screen isolation is diffusion and the migration of selecting precipitation and absorption effectively can stop radwaste.As with multilayered structure and there is the mineral substance of large pore volume volume and large specific surface area can by radwaste and pollutent, surface is adsorbed in as elements such as U, Np, Pu, to stop radionuclide to the Nature and biosphere migration particularly by actinide elements.
The mineral substance of phosphoric acid salt is due to its Heat stability is good, be insoluble in water, there are again a large amount of pore volumes and very large specific surface area, therefore some metal ion can optionally be adsorbed as ion-exchanger, there is the good exchange to metal and adsorption function, be highly suitable for process radio chemistry nuke rubbish.
Slaughter the reports such as Chengde and carry out a kind of synthetic method of zirconium phosphate (" the purification absorption novel material of core uranyl ion on crystalline zirconium phosphate ", " the 9th China's antibacterial industry development conference collection of thesis ", 2013, 209-214), in this synthetic method, the mol ratio of raw material phosphoric acid dihydro amine and zirconium oxychloride is 1:1, synthesis temperature is 1280 DEG C, be ground to grain diameter after roasting and be about 0.074 ㎜, adopt induction stirring 12 hours, use deionized water suction filtration again to washing electrical conductivity of water is the same with deionization electrical conductivity of water, last to dry 4 hours at 100 DEG C in an oven, thus obtain a kind of zirconium phosphate material.
A kind of preparation method of phosphoric acid salt mineral substance is prior art discloses although above-mentioned, certain needs can be met, but the method still exists some defects: such as, the ability of above-mentioned zirconium phosphate material absorption core uranium ion is still more weak, constrains its extensive use industrially.
Therefore, still there is further demand for the phosphoric acid salt mineral substance that can purify core uranium ion, this is also one of study hotspot and emphasis in this technical field, especially the power that is accomplished of the present invention and starting point place.
Summary of the invention
In order to the ability overcoming the zirconium phosphate absorption core uranium ion that prior art exists is more weak and then restrict the technical problem of industrial extensive use, the present inventor, after having carried out a large amount of further investigations, provides a kind of preparation method purifying the crystallization plastid zirconium phosphate of core uranium ion.
The present invention is achieved through the following technical solutions, and a kind of preparation method purifying the crystallization plastid zirconium phosphate of core uranium ion, comprises the following steps:
Step one, after phosphoric acid dihydro amine equal for mole number and zirconium oxychloride being mixed, 1216 ~ 1258 DEG C of roasting temperatures 1 ~ 4 hour;
Step 2, is ground to grain diameter and is about 0.07 ~ 0.08 ㎜, after induction stirring, then with deionized water suction filtration to washing electrical conductivity of water is the same with deionization electrical conductivity of water;
Step 3, finally dries 2 ~ 6 hours at 80 ~ 120 DEG C in an oven, to obtain final product.
Wherein, maturing temperature scope in step one 1216 ~ 1258 DEG C includes any concrete point value belonged to wherein, such as 1216 DEG C, 1217 DEG C, 1218 DEG C, 1219 DEG C, 1220 DEG C, 1223 DEG C, 1225 DEG C, 1228 DEG C, 1230 DEG C, 1232 DEG C, 1235 DEG C, 1240 DEG C, 1245 DEG C, 1247 DEG C, 1250 DEG C, 1253 DEG C, 1254 DEG C, 1255 DEG C, 1256 DEG C, 1257 DEG C, 1258 DEG C, most preferably 1235 DEG C, also include the scope that any two point values in these concrete point values are formed, preferably 1223 ~ 1247 DEG C.
Compared with prior art, beneficial effect of the present invention is as follows: the present invention is by optimizing maturing temperature and roasting time, thus make the crystallization plastid zirconium phosphate of synthesis further increase the ability of absorption core uranium ion, be more applicable to for disposing radio chemistry nuke rubbish.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art and understand the present invention further, but not limit the present invention in any form.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, some distortion and improvement can also be made.These all belong to protection scope of the present invention.
embodiment 1
The present embodiment relates to a kind of preparation method of crystallization plastid zirconium phosphate, comprises the following steps:
Step one, after phosphoric acid dihydro amine equal for mole number and zirconium oxychloride being mixed, 1235 DEG C of roasting temperatures 3 hours;
Step 2, is ground to grain diameter and is about 0.08 ㎜, after induction stirring, then with deionized water suction filtration to washing electrical conductivity of water is the same with deionization electrical conductivity of water;
Step 3, finally dries 3 hours at 80 DEG C in an oven, to obtain final product.
embodiment 2
The present embodiment relates to a kind of preparation method of crystallization plastid zirconium phosphate, comprises the following steps:
Step one, after phosphoric acid dihydro amine equal for mole number and zirconium oxychloride being mixed, 1247 DEG C of roasting temperatures 4 hours;
Step 2, is ground to grain diameter and is about 0.07 ㎜, after induction stirring, then with deionized water suction filtration to washing electrical conductivity of water is the same with deionization electrical conductivity of water;
Step 3, finally dries 4 hours at 90 DEG C in an oven, to obtain final product.
embodiment 3
The present embodiment relates to a kind of preparation method of crystallization plastid zirconium phosphate, comprises the following steps:
Step one, after phosphoric acid dihydro amine equal for mole number and zirconium oxychloride being mixed, 1258 DEG C of roasting temperatures 1 hour;
Step 2, is ground to grain diameter and is about 0.072 ㎜, after induction stirring, then with deionized water suction filtration to washing electrical conductivity of water is the same with deionization electrical conductivity of water;
Step 3, finally dries 5 hours at 100 DEG C in an oven, to obtain final product.
embodiment 4
The present embodiment relates to a kind of preparation method of crystallization plastid zirconium phosphate, comprises the following steps:
Step one, after phosphoric acid dihydro amine equal for mole number and zirconium oxychloride being mixed, 1216 DEG C of roasting temperatures 2 hours;
Step 2, is ground to grain diameter and is about 0.075 ㎜, after induction stirring, then with deionized water suction filtration to washing electrical conductivity of water is the same with deionization electrical conductivity of water;
Step 3, finally dries 6 hours at 110 DEG C in an oven, to obtain final product.
embodiment 5
The present embodiment relates to a kind of preparation method of crystallization plastid zirconium phosphate, comprises the following steps:
Step one, after phosphoric acid dihydro amine equal for mole number and zirconium oxychloride being mixed, 1223 DEG C of roasting temperatures 2.5 hours;
Step 2, is ground to grain diameter and is about 0.078 ㎜, after induction stirring, then with deionized water suction filtration to washing electrical conductivity of water is the same with deionization electrical conductivity of water;
Step 3, finally dries 2 hours at 120 DEG C in an oven, to obtain final product.
Comparative example 1
This comparative example is with the difference of embodiment 1: in step one, maturing temperature is 1200 DEG C.
Comparative example 2
This comparative example is with the difference of embodiment 1, and in step one, maturing temperature is 1205 DEG C.
Comparative example 3
This comparative example is with the difference of embodiment 1, and in step one, maturing temperature is 1210 DEG C.
Comparative example 4
This comparative example is with the difference of embodiment 1, and in step one, maturing temperature is 1213 DEG C.
Comparative example 5
This comparative example is with the difference of embodiment 1, and in step one, maturing temperature is 1260 DEG C.
Comparative example 6
This comparative example is with the difference of embodiment 1, and in step one, maturing temperature is 1265 DEG C.
Comparative example 7
This comparative example is with the difference of embodiment 1, and in step one, maturing temperature is 1270 DEG C.
Comparative example 8
This comparative example is with the difference of embodiment 1, and in step one, maturing temperature is 1275 DEG C.
Comparative example 9
This comparative example is with the difference of embodiment 1, and in step one, maturing temperature is 1280 DEG C.
adsorption test
Implement above-described embodiment 1-5 and comparative example 1-9 respectively, in the polyethylene centrifuge tube that 20ml is different, add the pressed powder of 150mg above-described embodiment and comparative example acquisition respectively, then adding 1.0ml concentration is 2.04 × 10
-3mol/L uranium nitrate solion and weight percent concentration are the potassium nitrate solution 1ml of 5%, then add 1ml organic acid fulvic acid, and organic acid concentration is 1.0 × 10
-4mol/L, adding water maintenance absorption system cumulative volume is 20ml, shakes 30 hours at 25 DEG C; Take out centrifugal 30 minutes, obtain supernatant liquor, the Mono Chloro Acetic Acid-sodium hydrate buffer solution then getting the above-mentioned supernatant liquor of 5.0ml and 1.0ml pH2.8 adds in the volumetric flask of 50ml, and the constant volume that adds water, finally under 652nm, survey its absorbancy.Absorption percentage ratio (Y) is: Y=(A
0-A)/A
0× 100%, wherein A
0for the absorbancy of uranium nitrate, A is the absorbancy of the solution after absorption.The absorbance detection of each embodiment and comparative example in triplicate, then gets its mean value, and acquired results is as shown in table 1 below.
The absorption result of table 1 embodiment 1-5 and comparative example 1-9
As seen from the above table, when maturing temperature≤1213 DEG C or >=1260 DEG C, absorption percentage ratio is all no more than 80%, be up to 75.3% (see comparative example 1-9), and when maturing temperature is 1216 ~ 1258 DEG C of these scopes, absorption percentage ratio is all greater than 85%, minimum is 85.4% (see embodiment 1-5), the amplification of absorption percentage ratio is obvious, make us beyond expectation, especially in embodiment 1, maturing temperature is 1235 DEG C time, absorption percentage ratio, up to 98.1%, can be used as best embodiment.This illustrates that maturing temperature has vital impact for the performance of final product absorption core uranium ion when adopting phosphoric acid dihydro amine and zirconium oxychloride synthesis preparation crystallization plastid zirconium phosphate.
Above specific embodiments of the invention are described.It is to be appreciated that the present invention is not limited to above-mentioned particular implementation, those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (4)
1. purify a preparation method for the crystallization plastid zirconium phosphate of core uranium ion, it is characterized in that, comprise the following steps:
Step one, after phosphoric acid dihydro amine equal for mole number and zirconium oxychloride being mixed, 1216 ~ 1258 DEG C of roasting temperatures 1 ~ 4 hour;
Step 2, being ground to grain diameter is 0.07 ~ 0.08 ㎜, after induction stirring, then with deionized water suction filtration to washing electrical conductivity of water is the same with deionization electrical conductivity of water;
Step 3, finally dries 2 ~ 6 hours at 80 ~ 120 DEG C in an oven, obtains crystallization plastid zirconium phosphate.
2. the preparation method of the crystallization plastid zirconium phosphate of purification core uranium ion as claimed in claim 1, it is characterized in that, in step one, maturing temperature is 1223 ~ 1247 DEG C.
3. the preparation method of the crystallization plastid zirconium phosphate of purification core uranium ion as claimed in claim 2, it is characterized in that, in step one, maturing temperature is 1235 DEG C.
4. the application of the crystallization plastid zirconium phosphate described in any one of claims 1 to 3 in purification core uranium ion.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108654580A (en) * | 2018-05-22 | 2018-10-16 | 南京理工大学 | A kind of order mesoporous zirconium phosphate material, preparation method and its application in waste water |
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| CN1470456A (en) * | 2002-07-26 | 2004-01-28 | 中国科学院大连化学物理研究所 | Zirconium phosphate crystal, and its preparing method and use |
| CN101602512A (en) * | 2009-07-18 | 2009-12-16 | 太原理工大学 | A kind of Zirconium phosphate crystal material and preparation method |
| CN102180455A (en) * | 2011-05-23 | 2011-09-14 | 大连交通大学 | Method for preparing sodium hydrogen zirconium phosphate powder |
-
2014
- 2014-10-08 CN CN201410524251.XA patent/CN104250002A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1470456A (en) * | 2002-07-26 | 2004-01-28 | 中国科学院大连化学物理研究所 | Zirconium phosphate crystal, and its preparing method and use |
| CN101602512A (en) * | 2009-07-18 | 2009-12-16 | 太原理工大学 | A kind of Zirconium phosphate crystal material and preparation method |
| CN102180455A (en) * | 2011-05-23 | 2011-09-14 | 大连交通大学 | Method for preparing sodium hydrogen zirconium phosphate powder |
Non-Patent Citations (1)
| Title |
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| 屠承德 等: ""核铀酰离子在结晶质磷酸锆上的净化吸附新材料"", 《第九届中国抗菌产业发展大会论文集》, 31 December 2013 (2013-12-31) * |
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| CN108654580A (en) * | 2018-05-22 | 2018-10-16 | 南京理工大学 | A kind of order mesoporous zirconium phosphate material, preparation method and its application in waste water |
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