阅读说明：本技术 一种六氟化铀制备八氧化三铀的方法及装置 (Method and device for preparing triuranium octoxide from uranium hexafluoride ) 是由 文金旋 杨晨 于 2021-08-16 设计创作，主要内容包括：本发明涉及核燃料制备技术领域,具体涉及一种六氟化铀制备八氧化三铀的方法及装置,通过取固体UF-(6)放入试管中,对试管进行加热,固定UF-(6)发生气化；将气化的UF-(6)导入水淋洗设备中进行水解反应,制备得到UO-(2)F-(2)溶液；将UO-(2)F-(2)导入试管中,将试管中加入浓度为30％的双氧水,搅拌混合液；将反应后的溶液放置于蒸发器内,加热浓缩为UO-(2)F-(2)结晶；将UO-(2)F-(2)结晶加工为UO-(2)F-(2)的粉末；将干燥的UO-(2)F-(2)粉末放入含有O-(2)的焙烧炉中,U-(3)O-(8)被氧化为U-(3)O-(8),如此,通过将六氟化铀放入试管中进行气化、水解、结晶和焙烧后,制得八氧化三铀,从而缩短了六氟化铀制备八氧化三铀的流程。(The invention relates to the technical field of nuclear fuel preparation, in particular to a method and a device for preparing triuranium octoxide from uranium hexafluoride by taking solid UF 6 Placing into test tube, heating the test tube, and fixing UF 6 Gasification occurs; UF to be gasified 6 Introducing the mixture into water leaching equipment for hydrolysis reaction to prepare UO 2 F 2 A solution; mixing UO 2 F 2 Introducing into a test tube, adding 30% hydrogen peroxide into the test tube, and stirring the mixed solution; placing the reacted solution in an evaporator, heating and concentrating to obtain UO 2 F 2 Crystallizing; mixing UO 2 F 2 Crystallization processing into UO 2 F 2 The powder of (4); drying the UO 2 F 2 The powder is put into a container containing O 2 In the roasting furnace, U 3 O 8 Is oxidized into U 3 O 8 Thus, uranium hexafluoride is put into a test tube for gasification and hydrolysisAnd crystallizing and roasting to prepare triuranium octoxide, thereby shortening the process of preparing triuranium octoxide from uranium hexafluoride.)

1. A method for preparing triuranium octoxide by uranium hexafluoride is characterized by comprising the following steps,

taking solid UF₆Placing into test tube, heating the test tube, and fixing UF₆Gasification occurs;

UF to be gasified₆Introducing the mixture into water leaching equipment for hydrolysis reaction to prepare UO₂F₂A solution;

mixing UO₂F₂Introducing into a test tube, adding 30% hydrogen peroxide into the test tube, and stirring the mixed solution;

placing the reacted solution in an evaporator, heating and concentrating to obtain UO₂F₂Crystallizing;

mixing UO₂F₂Crystallization processing into UO₂F₂The powder of (4);

drying the UO₂F₂The powder is put into a container containing O₂In a roasting furnace of (1), UO₂F₂Is oxidized into U₃O₈。

2. The method of claim 1 wherein UF is a solid removal process₆Placing into test tube, heating the test tube, and fixing UF₆In which gasification occurs, "the method further comprises,

cleaning the test tube and drying;

preheating the surface of the test tube by using an alcohol lamp;

subjecting the solid to UF₆Placing into a test tube, heating the test tube with alcohol lamp, UF₆Vaporization occurs during the heating process.

3. Process for the preparation of triuranium octoxide from uranium hexafluoride according to claim 1, wherein UF "to be gasified" is₆Introducing the mixture into water leaching equipment for hydrolysis reaction to prepare UO₂F₂In solution ", the method further comprises,

connecting one end of the conduit to the mouth of the test tube;

extending the other end of the conduit into the water of the water leaching device;

UO obtained in collecting water leaching equipment₂F₂And (3) solution.

4. Method for preparing triuranium octoxide from uranium hexafluoride according to claim 1, wherein the UO is added₂F₂Introducing into a test tube, adding 30% hydrogen peroxide into the test tube, stirring the mixed solution, and stirring,

the obtained UO₂F₂Sucking out the solution by a pipette;

the UO in the pipette₂F₂Dripping the solution into a clean test tube;

30 percent hydrogen peroxide is dripped into the test tube while stirring.

5. The method for preparing triuranium octoxide from uranium hexafluoride of claim 1, wherein the reacted solution is placed in an evaporator and heated to concentrate the solution into UO₂F₂In the crystallization ", the method further comprises,

pouring the solution obtained by the reaction into a vessel of an evaporator, and sealing the evaporator;

adjusting the heating temperature of the evaporator, and keeping the temperature after the solution begins to precipitate crystals;

after the solution is finishedConcentrating and crystallizing, and taking out concentrated UO₂F₂And (4) crystallizing.

6. The method for preparing triuranium octoxide from uranium hexafluoride according to claim 5, wherein in the step of adjusting the heating temperature of the evaporator and maintaining the temperature after the solution starts to crystallize, the method further comprises,

slowly adjusting the heating temperature of the evaporator, generating HF gas in the evaporation process, and introducing the generated HF gas into a sodium hydroxide solution to prepare a byproduct potassium fluocyanide.

7. An apparatus for preparing triuranium octoxide from uranium hexafluoride, wherein the apparatus is prepared by the method for preparing triuranium octoxide from uranium hexafluoride according to claims 1 to 8.

Technical Field

The invention relates to the technical field of nuclear fuel preparation, in particular to a method and a device for preparing triuranium octoxide from uranium hexafluoride.

Background

Currently in the field of nuclear fuel circulation, depletion of UF is predominant₆Preparation of depleted UF for feedstock₄、UO₂、U₃O₈Three kinds of hydrofluoric acid are obtained as a byproduct. Among the three products, UF₄Will react with vapor in the air to generate HF corrosion container; in addition UO₂The powder is easy to self-ignite and must be UO₂The ceramic form is stored, but slow oxidation reactions still occur; and U₃O₈Although the density is minimum, the catalyst can be continuously converted into UO₂Or recycling of metallic uranium.

During the preparation of triuranium octoxide, usually UF of the gas is used₆React with water vapor to prepare UO₂F₂The powder is then prepared by a 'wet' ADU thermal decomposition reduction method or a 'dry' direct reduction method, but the wet process has long process flow, the generated wastewater is large, and the dry method is used for preparing UO₂Will be hydrofluorinated by HF to UF₄Hardening into blocks and adding UO₂The fluorine content in (1).

Disclosure of Invention

The invention aims to provide a method and a device for preparing triuranium octoxide from uranium hexafluoride, and aims to solve the technical problem that in the prior art, the operation of preparing triuranium octoxide from uranium hexafluoride is complex due to excessive flows in the process of preparing triuranium octoxide.

In order to achieve the purpose, the invention adopts a method for preparing triuranium octoxide by uranium hexafluoride, which comprises the following steps,

taking solid UF₆Placing into test tube, heating the test tube, and fixing UF₆Gasification occurs;

UF to be gasified₆Introducing the mixture into water leaching equipment for hydrolysis reaction to prepare UO₂F₂A solution;

mixing UO₂F₂Introducing into a test tube, adding 30% hydrogen peroxide into the test tube, and stirring the mixed solution;

placing the reacted solution in an evaporator, heating and concentrating to obtain UO₂F₂Crystallizing;

mixing UO₂F₂Crystallization processing into UO₂F₂The powder of (4);

will dryDried UO₂F₂The powder is put into a container containing O₂In a roasting furnace of (1), UO₂F₂Is oxidized into U₃O₈。

Wherein, in the process of taking solid UF₆Placing into test tube, heating the test tube, and fixing UF₆In which gasification occurs, "the method further comprises,

cleaning the test tube and drying;

preheating the surface of the test tube by using an alcohol lamp;

subjecting the solid to UF₆Placing into a test tube, heating the test tube with alcohol lamp, UF₆Vaporization occurs during the heating process.

Wherein, in "UF to be gasified₆Introducing the mixture into water leaching equipment for hydrolysis reaction to prepare UO₂F₂In solution ", the method further comprises,

connecting one end of the conduit to the mouth of the test tube;

extending the other end of the conduit into the water of the water leaching device;

UO obtained in collecting water leaching equipment₂F₂And (3) solution.

Wherein, in₂F₂Introducing into a test tube, adding 30% hydrogen peroxide into the test tube, stirring the mixed solution, and stirring,

the obtained UO₂F₂Sucking out the solution by a pipette;

the UO in the pipette₂F₂Dripping the solution into a clean test tube;

30 percent hydrogen peroxide is dripped into the test tube while stirring.

Wherein, the solution after reaction is put in an evaporator and heated and concentrated into UO₂F₂In the crystallization ", the method further comprises,

pouring the solution obtained by the reaction into a vessel of an evaporator, and sealing the evaporator;

adjusting the heating temperature of the evaporator, and keeping the temperature after the solution begins to precipitate crystals;

after the solution is concentrated and crystallized, the concentrated UO is taken out₂F₂And (4) crystallizing.

Wherein in the step of regulating the heating temperature of the evaporator and keeping the temperature after the solution begins to precipitate crystals, the method further comprises the steps of,

slowly adjusting the heating temperature of the evaporator, generating HF gas in the evaporation process, and introducing the generated HF gas into a sodium hydroxide solution to prepare a byproduct potassium fluocyanide.

The invention also comprises a device for preparing triuranium octoxide from uranium hexafluoride, and the triuranium octoxide is prepared by adopting the method for preparing triuranium octoxide from uranium hexafluoride.

The invention discloses a method and a device for preparing triuranium octoxide from uranium hexafluoride, wherein solid UF is taken₆Placing into test tube, heating the test tube, and fixing UF₆Gasification occurs; UF to be gasified₆Introducing the mixture into water leaching equipment for hydrolysis reaction to prepare UO₂F₂A solution; mixing UO₂F₂Introducing into a test tube, adding 30% hydrogen peroxide into the test tube, and stirring the mixed solution; placing the reacted solution in an evaporator, heating and concentrating to obtain UO₂F₂Crystallizing; mixing UO₂F₂Crystallization processing into UO₂F₂The powder of (4); drying the UO₂F₂The powder is put into a container containing O₂In the roasting furnace, U₃O₈Is oxidized into U₃O₈So, put into the test tube through uranium hexafluoride and carry out gasification, hydrolysis, crystallization and calcination after, make triuranium octoxide to the flow of uranium hexafluoride preparation triuranium octoxide has been shortened.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.

FIG. 1 is a flow chart of the method for preparing triuranium octoxide from uranium hexafluoride according to the invention.

FIG. 2 is a solid UF of the present invention₆Placing into test tube, heating the test tube, and fixing UF₆Flow diagram of gasification occurring.

FIG. 3 is UF to be vaporized according to the invention₆Introducing the mixture into water leaching equipment for hydrolysis reaction to prepare UO₂F₂Flow chart of the solution.

FIG. 4 is a UO of the present invention₂F₂Introducing into a test tube, adding hydrogen peroxide solution with the concentration of 30% into the test tube, and stirring the mixed solution.

FIG. 5 shows the present invention in which the reacted solution is placed in an evaporator and heated to concentrate the solution into UO₂F₂The structure of the crystal is shown schematically.

FIG. 6 is a UO of the present invention₂F₂Crystallization processing into UO₂F₂Flow sheet of the powder of (1).

FIG. 7 is a UO of the present invention to be dried₂F₂The powder is put into a container containing O₂In a roasting furnace of (1), UO₂F₂Is oxidized into U₃O₈Is described.

Detailed Description

Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.

In the description of the present invention, it is to be understood that the terms "length", "width", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships illustrated in the drawings, and are used merely for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention. Further, in the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.

Referring to fig. 1 to 7, the present invention provides a method for preparing triuranium octoxide from uranium hexafluoride, including the following steps,

s101: taking solid UF₆Placing into test tube, heating the test tube, and fixing UF₆Gasification occurs;

s1011: cleaning the test tube and drying;

s1012: preheating the surface of the test tube by using an alcohol lamp;

s1013: subjecting the solid to UF₆Placing into a test tube, heating the test tube with alcohol lamp, UF₆Gasification occurs during heating;

in this embodiment, the sterilized transparent test tube is taken, washed and dried, and then solid UF is put in₆Before, after carrying out the centre gripping to the test tube through the test tube clamp, adopt the alcohol burner to preheat the surface of test tube, treat that the temperature is stable after, UF solid₆Placing into test tube, UF solid₆Heating, and fixing UF during heating₆Gasification takes place.

S102: UF to be gasified₆Introducing the mixture into water leaching equipment for hydrolysis reaction to prepare UO₂F₂A solution;

s1021: connecting one end of the conduit to the mouth of the test tube;

s1022: extending the other end of the conduit into the water of the water leaching device;

s1023: UO obtained in collecting water leaching equipment₂F₂A solution;

in this embodiment, UF is added as a solid₆After the test tube is placed, an air guide hose is installed at the opening of the test tube, the other end of the air guide hose extends into the water leaching equipment, and UF is fixed₆The gas generated by heating is led into a water spraying device through a gas guide hose for hydrolysis reaction, thereby obtaining UO₂F₂The solution of (1).

S103: mixing UO₂F₂Introducing into a test tube, adding 30% hydrogen peroxide into the test tube, and stirring the mixed solution;

s1031: the obtained UO₂F₂Sucking out the solution by a pipette;

s1032: the UO in the pipette₂F₂Dripping the solution into a clean test tube;

s1033: dropping 30% hydrogen peroxide into the test tube while stirring;

in this embodiment, UO produced in the water shower facility is subjected to₂F₂Sucking out the solution by using a pipette, wherein the pipette is a long-head needle tube with a balloon, the air in the pipette is discharged by squeezing the balloon part of the pipette, and then the end part of the long-head needle tube of the pipette is close to the prepared UO₂F₂The solution is dripped into a clean test tube after being absorbed, then 10ml of 30% hydrogen peroxide is added into the test tube, and the solution in the test tube is stirred while the hydrogen peroxide is dripped.

S104: placing the reacted solution in an evaporator, heating and concentrating to obtain UO₂F₂Crystallizing;

s1041: pouring the solution obtained by the reaction into a vessel of an evaporator, and sealing the evaporator;

s1042: slowly adjusting the heating temperature of the evaporator, generating HF gas in the evaporation process, and introducing the generated HF gas into a sodium hydroxide solution to prepare a byproduct potassium fluocyanide;

s1043: after the solution is concentrated and crystallized, the concentrated UO is taken out₂F₂Crystallizing;

in the embodiment, the mixed solution obtained by the reaction is poured into a vessel in an evaporator from a test tube, and after the solution is stood still, an opening door of the evaporator is closed, so that the interior of the evaporator is sealed; adjusting the internal temperature of the evaporator by knob, slowly heating to 130-170 deg.C, and heating and concentrating the solution to UO₂F₂Crystallizing and evaporating HF gas during heating, and passing the HF gas through sodium hydroxide solution to produce potassium fluorocyanide as a byproduct.

S105: mixing UO₂F₂Crystallization processing into UO₂F₂The powder of (4);

s1051: the obtained UO₂F₂Drying the crystals;

s1052: drying the UO₂F₂Putting the crystals into a milling tank;

s1053: by rolling the roller pair UO₂F₂Repeatedly rolling the crystals to obtain UO₂F₂The powder of (4);

in this embodiment, UO is obtained by₂F₂Drying the crystals, and after drying, subjecting the UO to crystallization₂F₂Grinding the crystals into powder in a grinding tank, wherein the grinding process requires repeated grinding by using a grinding roller, so that the obtained UO is obtained₂F₂The powder meets the requirements.

S106: drying the UO₂F₂The powder is put into a container containing O₂In a roasting furnace of (1), UO₂F₂Is oxidized into U₃O₈；

S1061: drying the UO₂F₂Putting the powder into a vessel of a roasting furnace;

s1062: filling O into the vessel of the roasting furnace₂Sealing;

s1063: adjusting the roasting temperature to 800 ℃, and heating 10Min per time to the UO in the vessel₂F₂The powder is stirred.

In the present embodiment, the obtained dried UO is used₂F₂Putting the powder into a vessel in a roasting furnace, and filling O into the vessel₂Post-sealing, by adjusting the baking temperature to 800 ℃ and maintaining the dried UO₂F₂Finally roasting the powder in a high-temperature aerobic environment to obtain black uranium oxide powder, namely U₃O₈。

The device for preparing the triuranium octoxide from the uranium hexafluoride is prepared by the method for preparing the triuranium octoxide from the uranium hexafluoride.

In this embodiment, the device for preparing triuranium octoxide from uranium hexafluoride is a test tube, a water leaching device, a heating and concentrating device and a roasting furnace, so that triuranium octoxide is prepared from uranium hexafluoride.

While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.