CN113218154A - Microwave drying UF4Method - Google Patents
Microwave drying UF4Method Download PDFInfo
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- CN113218154A CN113218154A CN202011314028.4A CN202011314028A CN113218154A CN 113218154 A CN113218154 A CN 113218154A CN 202011314028 A CN202011314028 A CN 202011314028A CN 113218154 A CN113218154 A CN 113218154A
- Authority
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- China
- Prior art keywords
- drying
- stage
- microwave
- water
- uranium tetrafluoride
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000001035 drying Methods 0.000 title claims abstract description 91
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- MZFRHHGRNOIMLW-UHFFFAOYSA-J uranium(4+);tetrafluoride Chemical compound F[U](F)(F)F MZFRHHGRNOIMLW-UHFFFAOYSA-J 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000012065 filter cake Substances 0.000 claims abstract description 17
- 239000012535 impurity Substances 0.000 claims abstract description 9
- 230000000704 physical effect Effects 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000005070 sampling Methods 0.000 claims abstract description 7
- 238000005520 cutting process Methods 0.000 claims abstract description 6
- 238000007599 discharging Methods 0.000 claims abstract description 6
- 239000000047 product Substances 0.000 claims abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 30
- 239000007789 gas Substances 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- 230000001681 protective effect Effects 0.000 claims description 15
- 238000011068 loading method Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 230000009467 reduction Effects 0.000 claims description 3
- 239000000843 powder Substances 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 3
- KCKICANVXIVOLK-UHFFFAOYSA-L dioxouranium(2+);difluoride Chemical compound [F-].[F-].O=[U+2]=O KCKICANVXIVOLK-UHFFFAOYSA-L 0.000 abstract description 2
- OOAWCECZEHPMBX-UHFFFAOYSA-N oxygen(2-);uranium(4+) Chemical compound [O-2].[O-2].[U+4] OOAWCECZEHPMBX-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- FCTBKIHDJGHPPO-UHFFFAOYSA-N uranium dioxide Inorganic materials O=[U]=O FCTBKIHDJGHPPO-UHFFFAOYSA-N 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 238000000108 ultra-filtration Methods 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 238000005485 electric heating Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003345 natural gas Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005049 combustion synthesis Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000644 propagated effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- SANRKQGLYCLAFE-UHFFFAOYSA-H uranium hexafluoride Chemical compound F[U](F)(F)(F)(F)F SANRKQGLYCLAFE-UHFFFAOYSA-H 0.000 description 1
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B3/00—Drying solid materials or objects by processes involving the application of heat
- F26B3/32—Drying solid materials or objects by processes involving the application of heat by development of heat within the materials or objects to be dried, e.g. by fermentation or other microbiological action
- F26B3/34—Drying solid materials or objects by processes involving the application of heat by development of heat within the materials or objects to be dried, e.g. by fermentation or other microbiological action by using electrical effects
- F26B3/347—Electromagnetic heating, e.g. induction heating or heating using microwave energy
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
- F26B25/22—Controlling the drying process in dependence on liquid content of solid materials or objects
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Microbiology (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Biotechnology (AREA)
- Molecular Biology (AREA)
- Drying Of Solid Materials (AREA)
Abstract
The invention belongs to the technical field of nuclear chemical powder preparation, and particularly relates to microwave drying UF4The method comprises a first stage of drying, wherein a precipitated uranium tetrafluoride filter cake is loaded into a material boat and weighed, the weight and the material thickness of the loaded uranium tetrafluoride filter cake are recorded, the uranium tetrafluoride filter cake is placed into a microwave oven, the power, the temperature and the time are set, and most of free water is removed; and (3) second-stage drying: drying the material in a first stage to remove most of free water; second stage drying, removing residual free water and partial bound water; and (3) third-stage drying: and (4) removing residual bound water, cutting off the power, cooling and discharging when the set temperature and time are reached, and sampling and analyzing the water, impurities and physical property in the uranium tetrafluoride. The product prepared by the method has low water content, low uranium dioxide content and low uranyl fluoride content, and stable quality.
Description
Technical Field
The invention belongs to the technical field of nuclear chemical powder preparation, and particularly relates to microwave drying UF4A method.
Background
Uranium tetrafluoride is a suitable raw material for manufacturing uranium metal heat release elements, is a raw material for producing uranium hexafluoride by a dry method, and UF is fluorinated by fluorine gas4Preparing UF6The method of (2) is economically reasonable.
UF4The fused salt with other fluoride can be used as fuel of homogeneous phase reactor. Drying as Wet preparation UF4The necessary procedures of the method for drying the uranium tetrafluoride filter cake are various, common methods comprise electric heating drying, coal heating drying, natural gas heating drying and the like, and the traditional drying method is UF (ultra filtration) for wet production4In the process of drying and dehydrating the filter cake, partial byproducts are generated, so that the problems of byproducts, low purity and the like of the product exist.
Disclosure of Invention
In view of the above disadvantages, the present invention aims to provide a microwave drying UF4The microwave drying is a controllable process, the microwave can be deeply inserted into the material to quickly raise the central temperature of the material to fire and initiate combustion synthesis, the microwave is radially propagated from inside to outside to uniformly heat the whole material, and finally the sintering reaction is completed. The performance of the product meets the standard requirement by adjusting a series of parameters and adjusting the microwave power.
The technical scheme of the invention is as follows:
microwave drying UF4The method comprises the steps of drying in the first stage, loading a precipitated uranium tetrafluoride filter cake into a material boat, weighing, recording the weight and the material thickness of the loaded uranium tetrafluoride filter cake, placing the uranium tetrafluoride filter cake into a microwave oven, setting power, temperature and time, and removing most of free water;
and (3) second-stage drying:
drying the material in a first stage to remove most of free water; second stage drying, removing residual free water and partial bound water;
and (3) third-stage drying:
and (4) removing residual bound water, cutting off the power, cooling and discharging when the set temperature and time are reached, and sampling and analyzing the water, impurities and physical property in the uranium tetrafluoride.
In the three-stage drying process, the thickness of the material is 10-40 mm.
And in the first stage, drying is carried out, the protective gas is nitrogen, the microwave output power is 1-3 kW, and the drying time is 2-10 min.
The first-stage drying set temperature is 60-75 ℃.
And drying in the second stage, wherein the protective gas is nitrogen, the microwave output power is 2-6 kW, and the drying time is 2-10 min.
And the set drying temperature of the second stage is 70-85 ℃.
And in the third stage of drying, the protective gas is nitrogen, the microwave output power is 3-9 kW, and the drying time is 2-10 min.
And in the third stage, the drying set temperature is 80-95 ℃, and after power failure and temperature reduction, the product is naturally cooled, and a sample is taken for moisture, impurities and physical property analysis.
The invention has the beneficial effects that:
the method adopts a microwave drying mode to dry the uranium tetrafluoride filter cake. Compared with uranium tetrafluoride powder prepared by electric heating drying, coal heating drying, natural gas heating drying and other modes, the uranium tetrafluoride powder has the advantages of small product moisture content, small uranium dioxide content and small uranyl fluoride content, and stable quality. Table 1 compares conventional drying and microwave drying UF4And (5) comparing the results.
TABLE 1 calcination results of uranium tetrafluoride after conventional drying and microwave drying
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Microwave drying UF4The method comprises the following specific steps:
drying in the first stage: loading the precipitated uranium tetrafluoride filter cake into a material boat, weighing, recording the weight and the material thickness of the loaded uranium tetrafluoride filter cake, placing the uranium tetrafluoride filter cake into a microwave oven, setting the power, the temperature and the time, and removing most of free water;
and (3) second-stage drying:
drying the material in a first stage to remove most of free water; second stage drying, removing residual free water and partial bound water;
and (3) third-stage drying:
the remaining bound water was removed. And when the set temperature and time are reached, cutting off the power, cooling and discharging, and sampling to analyze the moisture, impurities and physical properties in the uranium tetrafluoride.
The thickness of the material in the three-stage drying process can be 10-40 mm.
The first stage is drying, protective gas is nitrogen, microwave output power is 1-3 kW, drying time is 2-10 min, and set temperature is 60-75 ℃.
And drying in the second stage, wherein the protective gas is nitrogen, the microwave output power is 2-6 kW, the drying time is 2-10 min, and the set temperature is 70-85 ℃.
And in the third stage of drying, the protective gas is nitrogen, the microwave output power is 3-9 kW, the drying time is 2-10 min, and the set temperature is 80-95 ℃. And after power failure and temperature reduction, naturally cooling, and sampling to analyze moisture, impurities and physical properties.
Example 1:
drying in the first stage:
loading the precipitated uranium tetrafluoride filter cake into a material boat, weighing, setting power, temperature and time, drying the material at the first stage, wherein the thickness of the material can be 15mm, the protective gas is nitrogen, the microwave output power is 2kW, the drying time is 5min, the set temperature is 65 ℃, and most of free water is removed;
the drying is carried out in the second stage,
the protective gas is nitrogen, the microwave output power is 5kW, the drying time is 3min, the set temperature is 75 ℃, and the residual free water and part of the combined water are removed;
and in the third stage, drying is carried out, wherein the protective gas is nitrogen, the microwave output power is 7kW, the drying time is 4min, the set temperature is 85 ℃, and the residual bound water is removed. And when the set temperature and time are reached, cutting off the power, cooling and discharging, and sampling to analyze the moisture, impurities and physical properties in the uranium tetrafluoride.
Example 2:
drying in the first stage:
loading the precipitated uranium tetrafluoride filter cake into a material boat, weighing, setting power, temperature and time, drying the material at the first stage, wherein the thickness of the material can be 25mm, the protective gas is nitrogen, the microwave output power is 3kW, the drying time is 7min, the set temperature is 60 ℃, and most of free water is removed;
drying in the second stage, wherein the protective gas is nitrogen, the microwave output power is 6kW, the drying time is 4min, the set temperature is 75 ℃, and the residual free water and part of bound water are removed;
and in the third stage, drying is carried out, wherein the protective gas is nitrogen, the microwave output power is 7kW, the drying time is 3min, the set temperature is 90 ℃, and the residual bound water is removed. And when the set temperature and time are reached, cutting off the power, cooling and discharging, and sampling to analyze the moisture, impurities and physical properties in the uranium tetrafluoride.
In the disclosed embodiments of the present invention, only methods related to the disclosed embodiments are referred to, and other methods may refer to general designs, and under the condition of no conflict, the same embodiment and different embodiments of the present invention may be combined with each other;
the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that are within the spirit and principle of the present invention are intended to be included in the scope of the present invention.
Claims (8)
1. Microwave drying UF4The method is characterized in that:
drying in the first stage, namely loading the precipitated uranium tetrafluoride filter cake into a material boat for weighing, recording the weight and the material thickness of the loaded uranium tetrafluoride filter cake, placing the uranium tetrafluoride filter cake into a microwave oven, setting power, temperature and time, and removing most of free water;
and (3) second-stage drying:
drying the material in a first stage to remove most of free water; second stage drying, removing residual free water and partial bound water;
and (3) third-stage drying:
and (4) removing residual bound water, cutting off the power, cooling and discharging when the set temperature and time are reached, and sampling and analyzing the water, impurities and physical property in the uranium tetrafluoride.
2. A microwave drying UF as defined in claim 14The method is characterized in that: in the three-stage drying process, the thickness of the material is 10-40 mm.
3. A microwave drying UF as defined in claim 24The method is characterized in that: and in the first stage, drying is carried out, the protective gas is nitrogen, the microwave output power is 1-3 kW, and the drying time is 2-10 min.
4. A microwave drying UF as defined in claim 34The method is characterized in that: the first-stage drying set temperature is 60-75 ℃.
5. A microwave drying UF as defined in claim 24The method is characterized in that: and drying in the second stage, wherein the protective gas is nitrogen, the microwave output power is 2-6 kW, and the drying time is 2-10 min.
6. A microwave dryer as claimed in claim 5Dry UF4The method is characterized in that: and the set drying temperature of the second stage is 70-85 ℃.
7. A microwave drying UF as defined in claim 24The method is characterized in that: and in the third stage of drying, the protective gas is nitrogen, the microwave output power is 3-9 kW, and the drying time is 2-10 min.
8. A microwave drying UF according to claim 7, wherein4The method is characterized in that: and in the third stage, the drying set temperature is 80-95 ℃, and after power failure and temperature reduction, the product is naturally cooled, and a sample is taken for moisture, impurities and physical property analysis.
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CN202011314028.4A CN113218154A (en) | 2020-11-20 | 2020-11-20 | Microwave drying UF4Method |
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CN202011314028.4A CN113218154A (en) | 2020-11-20 | 2020-11-20 | Microwave drying UF4Method |
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Citations (14)
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---|---|---|---|---|
US4221680A (en) * | 1976-07-29 | 1980-09-09 | United Kindgom Atomic Energy Authority | Treatment of substances |
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-
2020
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Application publication date: 20210806 |