CN115924951A - Preparation method of calcium fluoride powder for cores - Google Patents
Preparation method of calcium fluoride powder for cores Download PDFInfo
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- CN115924951A CN115924951A CN202211649633.6A CN202211649633A CN115924951A CN 115924951 A CN115924951 A CN 115924951A CN 202211649633 A CN202211649633 A CN 202211649633A CN 115924951 A CN115924951 A CN 115924951A
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- reversing valve
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- cylinder
- calcium fluoride
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- 238000002360 preparation method Methods 0.000 title claims abstract description 91
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 title claims abstract description 42
- 229910001634 calcium fluoride Inorganic materials 0.000 title claims abstract description 42
- 239000000843 powder Substances 0.000 title claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 63
- 230000000694 effects Effects 0.000 claims abstract description 52
- 238000001914 filtration Methods 0.000 claims abstract description 42
- 238000001179 sorption measurement Methods 0.000 claims abstract description 33
- 238000002347 injection Methods 0.000 claims abstract description 9
- 239000007924 injection Substances 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 238000009833 condensation Methods 0.000 claims abstract description 6
- 230000005494 condensation Effects 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 78
- 238000001514 detection method Methods 0.000 claims description 52
- 238000006243 chemical reaction Methods 0.000 claims description 33
- 230000005540 biological transmission Effects 0.000 claims description 30
- 230000009471 action Effects 0.000 claims description 27
- 239000011148 porous material Substances 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 23
- 230000018044 dehydration Effects 0.000 claims description 22
- 238000006297 dehydration reaction Methods 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 21
- 239000012153 distilled water Substances 0.000 claims description 19
- 239000004744 fabric Substances 0.000 claims description 19
- 239000002994 raw material Substances 0.000 claims description 18
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 16
- 239000007787 solid Substances 0.000 claims description 15
- 239000002351 wastewater Substances 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 9
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 claims description 8
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 8
- 238000010521 absorption reaction Methods 0.000 claims description 7
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 5
- 230000000903 blocking effect Effects 0.000 claims description 5
- 229910052731 fluorine Inorganic materials 0.000 claims description 5
- 239000011737 fluorine Substances 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 230000010355 oscillation Effects 0.000 claims description 4
- 239000003507 refrigerant Substances 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 210000003437 trachea Anatomy 0.000 claims description 2
- 238000011010 flushing procedure Methods 0.000 claims 1
- 238000005096 rolling process Methods 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 7
- 230000006872 improvement Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000009795 derivation Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011343 solid material Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 229910052770 Uranium Inorganic materials 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 2
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 2
- 101100314150 Caenorhabditis elegans tank-1 gene Proteins 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- MZFRHHGRNOIMLW-UHFFFAOYSA-J uranium(4+);tetrafluoride Chemical compound F[U](F)(F)F MZFRHHGRNOIMLW-UHFFFAOYSA-J 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Images
Classifications
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Landscapes
- Removal Of Specific Substances (AREA)
- Separation Of Gases By Adsorption (AREA)
Abstract
The invention discloses a preparation method of nuclear calcium fluoride powder, which relates to the related field of calcium fluoride and comprises a preparation tank, wherein the top of the preparation tank is fixedly provided with a lower stock bin with a quantitative blanking function and a liquid injection port with a liquid injection function, a preparation assembly is arranged at the left end of the preparation tank, a multi-directional flow guide effect is provided for a preparation solution through a guide-out pump and a first reversing valve, each preparation step is intelligently controlled through a second reversing valve and other components, the intelligent control effect on the preparation steps is favorably improved, a gas filtering assembly is arranged at the left end of the preparation tank, the gas in the liquid is separated through the condensation effect of an adsorption inner cylinder and a heat exchange tube, and the gas-liquid separation effect is improved through the centrifugal force generated by the preparation solution under the rotational flow effect of a baffle.
Description
Technical Field
The invention relates to the field related to calcium fluoride, in particular to a preparation method of calcium fluoride powder for a core.
Background
Calcium fluoride is an inorganic compound with a chemical formula of CaF2, and is colorless crystal or white powder; is insoluble in water and slightly soluble in inorganic acid, and reacts with hot concentrated sulfuric acid to generate hydrofluoric acid; in the process of preparing uranium metal in the nuclear industry, a method for reducing uranium tetrafluoride by calcium is generally adopted, in order to avoid introducing impurities into the uranium metal caused by melting of a metal container at high temperature, calcium fluoride which is the same as a reaction byproduct is lined between a reaction material and the reaction metal container; the materials used as the refractory lining are various, such as calcium fluoride, graphite, magnesium oxide, calcium oxide and the like, and the calcium fluoride with high purity is selected as the refractory lining to be most ideal.
In the prior art, a plurality of preparation raw materials are mostly and directly added in proportion in the preparation process, the priority of the sequential reaction process of the plurality of raw materials is not sequenced, and a detection component for performing acid-base data on mixed liquid in the preparation process is also not available;
meanwhile, more equipment is needed in the preparation process in the prior art, so that the size of the whole device in the prior art is large, a large amount of manpower is needed for auxiliary addition and operation in the preparation process, the automation degree is poor, and the labor cost in the preparation process in the prior art is high.
Disclosure of Invention
Accordingly, in order to solve the above-mentioned disadvantages, the present invention provides a method for preparing calcium fluoride powder for a core.
The invention is realized in such a way, the device comprises a preparation tank, wherein the top of the preparation tank is fixedly provided with a blanking bin with the function of quantitative blanking and a liquid injection port with the function of liquid injection;
the preparation assembly comprises a discharge pump, and the preparation tank and the through hole at the bottom of the reaction tank are connected with a water inlet pipeline at the top of the discharge pump through connecting pipes; the pipeline of the water outlet at the rear end of the guide-out pump is provided with a first reversing valve which plays a role in guiding; the left end of the first reversing valve is fixedly provided with an air filtering component through a connecting pipe; the pipeline at the bottom of the air filtering assembly is provided with a second reversing valve which plays a role in control; the bottom of the second reversing valve is provided with a dehydration component for dehydration; the first external pipe is arranged on a water inlet pipeline at the rear end of the second reversing valve; the return pipe is arranged on the water outlet pipeline at the rear end of the first reversing valve and plays a role in returning; the rear end of the return pipe is provided with a detection component for detecting; the top of the detection assembly is provided with a second external connecting pipe; the quick connectors are arranged at the joints of the outer sides of the first external connecting pipe and the second external connecting pipe, and the guide pump, the first reversing valve and the second reversing valve are electrically connected with the controller.
Preferably, the air filtering assembly comprises a temperature control outer cylinder, and the top side of the left end of the preparation tank is fixedly provided with the temperature control outer cylinder; the inner side wall of the temperature control outer cylinder is fixedly provided with an adsorption inner cylinder which plays a role in separation and adsorption through bolts; the outer side wall of the adsorption inner cylinder is fixedly adhered with a heat exchange tube which plays a role in heat exchange; the water inlets and the water outlets on the upper side and the lower side of the heat exchange tube are connected with an external valve pipeline; the baffle plate which plays a role in stirring flow is fixedly welded on the inner side wall of the adsorption inner cylinder; the guide air pipe which plays a role in guiding flow is fixedly welded in the central through hole of the baffle; the pipeline at the top of the lead-out air pipe is provided with a quick connector; wherein, adsorb the inner tube inside wall and be equipped with the slot that plays the choked flow effect.
Preferably, the dehydration component comprises a dehydration cylinder, and a water cylinder for dehydration is fixedly arranged at the bottom side of the left end of the preparation tank; the bottom of the third reversing valve is arranged with the pipeline at the bottom of the first reversing valve through a connecting pipe; the bottom inside the dewatering cylinder is rotatably provided with the fine-pore filter cylinder with a filtering function through a bracket; the inner side wall of the fine-pore filter cylinder is fixedly adhered with the water filtering cloth which plays a role in filtering; the outer side of the connecting plate at the top of the fine-hole filter cylinder is provided with a toothed ring which plays a role in transmission through bolts; the outer side of the gear ring is meshed with the rear end of the transmission gear; the center hole of the transmission gear is connected with a transmission shaft key of the servo motor; the servo motor is installed inside the dewatering cylinder front side protection box through bolts, and the third reversing valve and the servo motor are electrically connected with the controller.
Preferably, the detection assembly comprises a connecting sleeve, and the connecting sleeve playing a role in guiding flow is installed on a pipeline at the rear end of the return pipe; the pipeline at the rear end of the connecting sleeve is provided with a fourth reversing valve which plays a role in guiding; the fourth reversing valve pipeline is arranged at the bottom of the detection cylinder; the pipeline at the top of the detection cylinder is provided with a fifth reversing valve which plays a role in guiding; the magnet vibrator is mounted at the left end of the detection cylinder through a bolt and plays a role in detection; the detector is mounted at the rear end of the detection cylinder through a bolt; the upper side of the front end of the detector is fixedly provided with a sample measuring electrode through a lead; the reference electrode is fixedly arranged on the lower side of the front end of the detector through a lead; and the fourth reversing valve, the fifth reversing valve, the magnet vibrator, the detector, the sample measuring electrode and the reference electrode are all electrically connected with the controller.
Preferably, the controller at preparation jar front side is installed to preparation tank deck middle part side bolt transmission motor and bolt, transmission motor bottom transmission shaft fixed mounting has the stirring rake that plays the stirring effect, the stirring rake rotates and sets up inside the retort, preparation jar front end bottom side is equipped with the hot water pipe.
Preferably, the baffle is spirally distributed on the inner wall of the adsorption inner cylinder, and the diameter of the central through hole of the baffle is equal to that of the guide-out air pipe.
Preferably, the filter screen diameters of the fine-pore filter cylinder and the water filter cloth are respectively 1 cm and 1 mm.
Preferably, the front end of the dewatering cylinder is provided with a connecting box body which plays a role in protecting the servo motor.
Preferably, the top of the fourth reversing valve and the bottom of the fifth reversing valve are both provided with second external connecting pipes, and the end heads of the two groups of second external connecting pipes are both provided with quick connectors.
Preferably, the preparation method of the calcium fluoride powder for the core comprises the following preparation steps:
quantitatively adding distilled water and ammonium bifluoride raw material: adding a certain amount of distilled water into a reaction tank in the preparation tank, introducing external hot water into the preparation tank through a hot water guide pipe, heating the distilled water in the reaction tank, keeping the distilled water at 60-80 ℃ through controlling the temperature of the external hot water, adding a certain amount of ammonium bifluoride raw material into the reaction tank, wherein the solid-liquid ratio of the ammonium bifluoride raw material to the distilled water is 1;
step two: quantitatively and slowly adding calcium carbonate raw materials: then, the calcium carbonate raw material is slowly and quantitatively led into the reaction tank through the vibration of a discharging bin and is dissolved by stirring, and the ratio of the calcium carbonate raw material to the mixed liquid is 1:7, keeping the interior of the reaction tank at 60-80 ℃ under the action of heat introduced by the hot water guide pipe, and fully reacting under the stirring action of the stirring paddle, wherein the mixed solution can be introduced into the detection assembly 28 for detection under the driving action of the guide-out pump 21 and the first reversing valve 22;
step three: leading out filtered gas: then the mixed liquid in the reaction tank is led out through the lead-out pump and flows into the absorption inner cylinder under the driving action of the first reversing valve, at the moment, the lead-out pump provides lead-out pressure for the liquid, so that the mixed liquid with reaction crystals forms a rotational flow state under the flow choking action of the baffle, and meanwhile, an external refrigerant is led into the heat exchange tube through the external valve, so that the heat of the whole absorption inner cylinder is taken away by the external refrigerant, the mixed liquid can be contacted with the inner wall of the absorption inner cylinder under the rotational flow centrifugal action, gas in the mixed liquid can be contacted with the absorption inner cylinder to be separated from the liquid due to the condensation action of the liquid, so that liquid particles can be attached to the inner side of the absorption inner cylinder, and are prevented from being taken away by airflow through groove strips on the inner side of the absorption inner cylinder, and the separation of hydrogen generated by the reaction in the mixed liquid is favorably improved;
step four: and (3) centrifugal dehydration: then the degassed mixed liquid is guided into the dewatering component under the action of a second reversing valve, the mixed liquid flowing in is collected through the fine-pore filter cylinder and the water filtering cloth, then the servo motor is controlled by the controller to drive the transmission gear to rotate and enable the transmission gear to be meshed with the toothed ring, so that the toothed ring drives the fine-pore filter cylinder and the water filtering cloth to rotate, and redundant fluorine-containing wastewater is separated from calcium fluoride solid through the filtering effect of the fine-pore filter cylinder and the water filtering cloth and the centrifugal force during rotation and is led out through a third reversing valve;
step five: and (4) repeating washing: external distilled water is guided into the fine-pore filter cylinder through the flow guide effect of the second reversing valve and the second external connecting pipe to wash and wash the calcium fluoride solid;
step six: and (3) detection of the pH value: at the moment, the washing wastewater is led into the first reversing valve due to the reversing effect of the third reversing valve, the washing wastewater flows into the detection cylinder through the reversing effect of the first reversing valve and the fourth reversing valve, the magnet vibrator is controlled by the controller to oscillate, the sample measuring electrode and the reference electrode generate detection data under the action of oscillation waves and transmit the data to the detector, the detector monitors the washing PH value through two sets of data, and the PH values of liquid and solid are kept consistent in the washing process, so that the PH value data of calcium fluoride solid is also obtained;
step seven: grinding to prepare powder: when the pH value data reaches the standard value, the repeated washing is stopped, and the calcium fluoride solid is taken out for drying and grinding.
The invention has the following advantages: the invention provides a preparation method of calcium fluoride powder for nucleus by improvement, compared with the same type of equipment, the preparation method comprises the following improvements:
according to the preparation method of the nuclear calcium fluoride powder, the preparation assembly is arranged at the left end of the preparation tank, the multi-directional flow guide effect is provided for the preparation solution through the guide pump and the first reversing valve, and the intelligent control on each preparation step is realized through the components such as the second reversing valve, so that the intelligent control effect on the preparation steps is favorably improved.
According to the preparation method of the nuclear calcium fluoride powder, the gas filtering assembly is arranged at the left end of the preparation tank, gas in liquid is separated through the condensation effect of the adsorption inner cylinder and the heat exchange tube, and the prepared solution generates centrifugal force through the rotational flow effect of the baffle plate so as to improve the gas-liquid separation effect.
According to the preparation method of the nuclear calcium fluoride powder, the dehydration component is arranged at the left end of the preparation tank, the fine-hole filter cylinder and the toothed ring are respectively driven to rotate at high speed through the servo motor, and the solid is blocked under the filtering action of the fine-hole filter cylinder and the water filtering cloth, so that the dehydration and washing effects of the solid material are improved.
The invention relates to a preparation method of calcium fluoride powder for nuclear, which is characterized in that a detection component is arranged at the rear side of a preparation tank, a detection cylinder and a return pipe can form a return closed loop under the reversing and flow guiding effects of a third reversing valve and a fourth reversing valve, and a magnet vibrator and a detector are used for detecting the pH value of prepared materials under the multiple data detection effects of a sample detection electrode and a reference electrode.
Drawings
FIG. 1 is a schematic flow chart of the steps of the present invention;
FIG. 2 is a schematic perspective view of a preparation tank and preparation assembly of the present invention;
FIG. 3 is a schematic perspective cross-sectional structural view of a preparation assembly of the present invention;
FIG. 4 is a schematic view of the internal structure of the air filter assembly of the present invention;
FIG. 5 is a schematic perspective view of an adsorption inner tube and a heat exchange tube according to the present invention;
FIG. 6 is a schematic perspective cross-sectional view of a dewatering assembly of the present invention;
FIG. 7 is a perspective view of the inspection assembly of the present invention;
fig. 8 is a schematic perspective exploded view of the inspection assembly of the present invention.
Wherein: the device comprises a preparation tank-1, a preparation component-2, a blanking bin-3, a liquid injection port-4, a transmission motor-5, a controller-6, a stirring paddle-7, a reaction tank-8, a hot water guide pipe-9, a lead-out pump-21, a first reversing valve-22, a gas filtering component-23, a second reversing valve-24, a dehydration component-25, a first external connecting pipe-26, a return pipe-27, a detection component-28, a second external connecting pipe-29, a temperature control external cylinder-231, an adsorption internal cylinder-232, a heat exchange pipe-233, an external valve-234, a baffle-235, a lead-out air pipe-236, a quick connector-237, a dehydration cylinder-251, a third reversing valve-252, a pore filter cylinder-253, a water filtering cloth-254, a gear ring-255, a transmission gear-256, a servo motor-257, a connecting sleeve-281, a fourth reversing valve-282, a detection cylinder-283, a fifth reversing valve-284, a magnet vibrator-285, a detector-287, a sample measuring electrode-287, and a reference electrode-288.
Detailed Description
The principles and features of the present invention are described below with reference to the accompanying drawings 1-8, which are given by way of illustration only and are not intended to limit the scope of the invention. The invention is described in more detail in the following paragraphs by way of example with reference to the accompanying drawings. Advantages and features of the present invention will become apparent from the following description and from the claims. It is to be noted that the drawings are in a very simplified form and are not to precise scale, which is provided for the purpose of facilitating and clearly illustrating embodiments of the present invention.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When a component is referred to as being "connected" to another component, it can be directly connected to the other component or intervening components may also be present. When a component is referred to as being "disposed on" another component, it can be directly on the other component or intervening components may also be present. The terms "vertical," "horizontal," "left," "right," and the like as used herein are for illustrative purposes only.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1-8, the method for preparing calcium fluoride powder for nuclear use of the present invention includes a preparation tank 1, a feed bin 3 for quantitative feeding and a liquid injection port 4 for liquid injection are fixedly installed on the top of the preparation tank 1, a transmission motor 5 and a controller 6 are installed on the front side of the preparation tank 1 by bolts, a stirring paddle 7 for stirring is fixedly installed on a transmission shaft at the bottom of the transmission motor 5, the stirring paddle 7 is rotatably installed inside a reaction tank 8, and a hot water conduit 9 is installed on the bottom side of the front end of the preparation tank 1.
The method is characterized in that: still including setting up the preparation subassembly 2 at preparation jar 1 left end, preparation subassembly 2 is including deriving pump 21, preparation jar 1 and 8 bottom through-holes of retort are all connected with derivation pump 21 top water inlet pipeline through the connecting pipe, derivation pump 21 rear end water outlet pipeline installs the first switching-over valve 22 that plays the guide effect, provide the switching-over effect for deriving pump 21 derivation direction through first switching-over valve 22, first switching-over valve 22 left end has gas filtering component 23 through connecting pipe fixed mounting, gas filtering component 23 bottom pipeline mounting has the second switching-over valve 24 that plays the control action, second switching-over valve 24 bottom is equipped with the dehydration subassembly 25 that plays the dehydration, second switching-over valve 24 rear end water inlet pipeline mounting has first external connecting pipe 26, the distilled water of washing usefulness is led in through first external connecting pipe 26, first switching-over valve 22 rear end water outlet pipeline mounting has the back flow 27 that plays the backward flow effect, the rear end of back flow 27 is equipped with the detection subassembly 28 that plays the detection effect, detection subassembly 28 top is equipped with second external connecting pipe 29, first external connecting pipe 26 and second external connecting pipe 29 all are equipped with the outside connecting joint 29, the first external connecting pipe 24 and second switching-over valve 24 all provide electric energy control for second switching-over pump 21 and second switching-over valve 22, the second switching-over valve 22.
The air filtering component 23 comprises an outer temperature control barrel 231, an outer temperature control barrel 231 is fixedly installed on the top side of the left end of the preparation tank 1, the inner side wall of the outer temperature control barrel 231 is fixedly provided with an adsorption inner barrel 232 with a separation and adsorption effect through bolts, a concentrated converging effect is provided for mixed liquid through the adsorption inner barrel 232, the outer side wall of the adsorption inner barrel 232 is fixedly adhered with a heat exchange tube 233 with a heat exchange effect, water inlets and water outlets on the upper side and the lower side of the heat exchange tube 233 are all connected with an external valve 234 through a pipeline, a baffle 235 with a flow stirring effect is fixedly welded on the inner side wall of the adsorption inner barrel 232, a rotational flow centrifugal effect is provided for liquid through the baffle 235, a guide-out air pipe 236 with a flow guiding effect is fixedly welded on the center through hole of the baffle 235, a quick joint 237 is installed on the top pipeline of the guide-out air pipe 236, a groove with a flow blocking effect is arranged on the inner side wall of the adsorption inner barrel 232, and a flow blocking effect is provided for water drops on the inner side wall of the adsorption inner barrel 232 through the groove.
The dehydration component 25 comprises a dehydration cylinder 251, a water cylinder 251 playing a role in dehydration is fixedly installed at the bottom side of the left end of the preparation tank 1, a third reversing valve 252 is installed at a water outlet pipeline at the bottom of the dehydration cylinder 251, a reversing effect is provided for washing wastewater through the third reversing valve 252, the bottom of the third reversing valve 252 is installed with a pipeline at the bottom of the first reversing valve 22 through a connecting pipe, a pore filter cylinder 253 playing a role in filtration is rotatably arranged at the bottom inside the dehydration cylinder 251 through a support, filter cloth 254 playing a role in filtration is fixedly adhered to the inner side wall of the pore filter cylinder 253, filter flow blocking effect is provided through the pore filter cylinder 253 and the filter cloth 254, a toothed ring 255 playing a role is installed on the outer side of the connecting plate at the top of the pore filter cylinder 253 through a bolt, the outer side of the toothed ring 255 is meshed with the rear end of a transmission gear 256, the center hole of the transmission gear 256 is connected with a transmission shaft of a servo motor 257, transmission force is provided for the transmission gear 256 through the servo motor 257, the servo motor 257 bolt is installed inside a protection box at the front side of the dehydration cylinder 251, the third reversing valve 252 and the servo motor 257 are electrically connected with a controller 6.
The detection assembly 28 comprises a connecting sleeve 281, the connecting sleeve 281 playing a role in guiding is installed on a rear end pipeline of the return pipe 28, a fourth reversing valve 282 playing a role in guiding is installed on a rear end pipeline of the connecting sleeve 281, the fourth reversing valve 282 is installed on the bottom of the detection cylinder 283 in a pipeline manner, a fifth reversing valve 284 playing a role in guiding is installed on the top of the detection cylinder 283 in a pipeline manner, a closed loop circulation effect is provided for the detection cylinder 283 through the fourth reversing valve 282 and the fifth reversing valve 284, the magnet 285 oscillator 283 is installed on the left end of the detection cylinder 283 in a bolt manner, the detector 286 is installed on the rear end of the detection cylinder 283 in a bolt manner, the sample electrode 287 is fixedly installed on the upper side of the front end of the detector 286 through a lead wire, the reference electrode 288 is fixedly installed on the lower side of the front end of the detector 286 through a lead wire, the fourth reversing valve 282, the fifth reversing valve 284, the magnet 285, the detector 286, the sample electrode 287 and the reference electrode 288 are electrically connected with the controller 6, and the fourth reversing valve 282, the fifth reversing valve 284, the magnet 285, the detector 286, the sample electrode 287 and the reference electrode 288 are electrically connected with the reference electrode 288.
Baffle 235 is the heliciform and distributes in the inner wall department that adsorbs inner tube 232, and baffle 235 central through-hole diameter with derive trachea 236, provides the whirl effect for adsorbing the inside liquid of inner tube 232 through baffle 235.
The mesh diameters of the fine-meshed filter cartridge 253 and the water filtering cloth 254 are 1 cm and 1 mm, respectively, and the filtering effect for the prepared solution is provided by the fine-meshed filter cartridge 253 and the water filtering cloth 254.
The front end of the dewatering cylinder 251 is provided with a connecting box body which plays a protection role for the servo motor 257, and the servo motor 257 is provided with a protection effect through the connecting box body.
The top of the fourth direction valve 282 and the bottom of the fifth direction valve 284 are both provided with a second external connection pipe 29, and the end heads of the two sets of second external connection pipes 29 are both provided with a quick coupling, so that the second external connection pipe 29 provides a liquid guiding effect for the fourth direction valve 282 and the fifth direction valve 284.
The invention provides a preparation method of calcium fluoride powder for nucleus by improvement, and the working principle is as follows;
firstly, when the equipment is used, the equipment is placed in a working area, and then a device is connected with an external power supply, so that the power supply required by the work of the equipment can be provided;
secondly, when the preparation is carried out, a worker adds a certain amount of distilled water into a reaction tank 8 in a preparation tank 1, then introduces external hot water into the preparation tank 1 through a hot water guide pipe 9, heats the distilled water in the reaction tank 8, keeps the distilled water at 60-80 ℃ through controlling the temperature of the external hot water, then enters the reaction tank 8 through adding a certain amount of ammonium bifluoride raw material, wherein the solid-liquid ratio of the ammonium bifluoride raw material to the distilled water is 1;
thirdly, the calcium carbonate raw material is then slowly and quantitatively introduced into the interior of the reaction tank 8 by vibration of the discharge bin 3 and dissolved by stirring, where the ratio of the calcium carbonate raw material to the mixed liquid is 1:7, keeping the interior of the reaction tank 8 at 60-80 ℃ under the action of heat conducted by the hot water conduit 9, fully reacting under the stirring action of the stirring paddle 7, introducing the mixed solution into a detection assembly (28) for detection under the driving action of a lead-out pump (21) and a first reversing valve (22), and then leading out the mixed liquid in the reaction tank 8 through the lead-out pump 21 and making the mixed liquid flow into the adsorption inner cylinder 232 under the driving action of the first reversing valve (22);
fourthly, at the moment, the guide pump 21 provides guide pressure for the liquid, so that the mixed liquid with reaction crystals forms a rotational flow state under the flow choking action of the baffle 235, meanwhile, an external refrigerant is guided into the heat exchange tube 233 through the external valve 234, so that the heat of the whole adsorption inner tube 232 is taken away by the mixed liquid, the mixed liquid can be contacted with the inner wall of the adsorption inner tube 232 under the rotational flow centrifugal action, and thus, the gas in the mixed liquid can be contacted with the adsorption inner tube 232 to be separated from the liquid due to the condensation action of the liquid, so that liquid particles can be attached to the inner side of the adsorption inner tube 232, and can be prevented from being taken away by air flow through groove strips on the inner side of the adsorption inner tube 232, and the separation of hydrogen generated by the reaction in the mixed liquid can be improved;
fifthly, introducing the degassed mixed liquid into the dewatering component 25 under the action of the second reversing valve 24, collecting the introduced mixed liquid through the fine-pore filter cylinder 253 and the water filtering cloth 254, controlling the servo motor 257 to drive the transmission gear 256 to rotate and enable the transmission gear 256 to be meshed with the toothed ring 255, so that the toothed ring 255 drives the fine-pore filter cylinder 253 and the water filtering cloth 254 to rotate, separating redundant fluorine-containing wastewater from calcium fluoride solids through the filtering effect of the fine-pore filter cylinder 253 and the water filtering cloth 254 and the centrifugal force during rotation, leading out the redundant fluorine-containing wastewater through the third reversing valve 252, and introducing external distilled water into the fine-pore filter cylinder 253 to flush and wash the calcium fluoride solids through the flow guiding effect of the second reversing valve 24 and the second external connecting pipe 29;
sixthly, at this time, the washing wastewater is introduced into the first reversing valve 22 by the reversing effect of the third reversing valve 252, the washing wastewater flows into the detection cylinder 283 by the reversing effect of the first reversing valve 22 and the fourth reversing valve 282, the magnet vibrator 285 is controlled by the controller 6 to perform oscillation operation, the sample measuring electrode 287 and the reference electrode 288 are subjected to oscillation wave to generate detection data, and the data are transmitted to the detector 286, the detector 286 monitors the washing pH value by two sets of data, and the pH values of liquid and solid are consistent during the washing process, so that the pH value data of calcium fluoride solid is also obtained, meanwhile, external distilled water can be introduced through the second external connecting pipe 29 to clean the components such as the sample measuring electrode 287 and the reference electrode 288, and the like, so that the influence of data among multiple detections is reduced, and the interior of the reaction tank 8 can be flushed by the washing wastewater which is gradually diluted; when the pH value data reaches the standard value, the repeated washing is stopped, and the calcium fluoride solid is taken out for drying and grinding.
The invention provides a preparation method of calcium fluoride powder for nuclear by improvement, which is characterized in that a preparation component 2 is arranged at the left end of a preparation tank 1, a multi-directional flow guide effect is provided for a preparation solution by a lead-out pump 21 and a first reversing valve 22, each preparation step is intelligently controlled by a second reversing valve 24 and other components, the intelligent control effect on the preparation steps is favorably improved, a gas-liquid separation effect is improved by arranging a gas filtering component 23 at the left end of the preparation tank 1, gas in liquid is separated by the condensation effect of an adsorption inner cylinder 232 and a heat exchange tube 233, the preparation solution generates centrifugal force by the rotational flow effect of a baffle plate 235, the dehydration and washing effects on solid materials are favorably improved by arranging a dehydration component 25 at the left end of the preparation tank 1, a pore 253 and a toothed ring 255 are respectively driven to rotate at high speed by a servo motor 257, solids are blocked by the filtering effect of a pore filter cylinder 253 and a water filtering cloth 254, the dehydration and washing effects on the solid materials are favorably improved, a detection component 28 is arranged at the rear side of the preparation tank 1, a detection component 283 and a magnet return flow detector 285 and a closed loop electrode detection component 288 are used for detecting the backflow value of a magnet through the operation vibrator 288 and a pH detection component 285.
The basic principles and main features of the present invention and the advantages of the present invention are shown and described above, and the standard parts used in the present invention can be purchased from the market, the special-shaped parts can be customized according to the description and the description of the attached drawings, the specific connection mode of each part adopts the conventional means of bolt, rivet, welding and the like mature in the prior art, the machinery, parts and equipment adopt the conventional type in the prior art, and the circuit connection adopts the conventional connection mode in the prior art, and the details are not described herein.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A preparation device of calcium fluoride powder for nuclear comprises a preparation tank (1), wherein the top of the preparation tank (1) is fixedly provided with a blanking bin (3) playing a role in quantitative blanking and a liquid injection port (4) playing a role in liquid injection;
the method is characterized in that: still including setting up preparation subassembly (2) at preparation jar (1) left end, preparation subassembly (2) include:
the through holes at the bottoms of the preparation tank (1) and the reaction tank (8) are connected with a water inlet pipeline at the top of the discharge pump (21) through connecting pipes;
the water outlet pipeline at the rear end of the guide pump (21) is provided with a first reversing valve (22) with a guiding function;
the left end of the first reversing valve (22) is fixedly provided with the air filtering assembly (23) through a connecting pipe;
the second reversing valve (24) is arranged on a pipeline at the bottom of the air filtering assembly (23) and plays a role in control;
the bottom of the second reversing valve (24) is provided with a dewatering component (25) for dewatering;
a first external pipe (26), wherein a first external pipe (26) is installed on a water inlet pipeline at the rear end of the second reversing valve (24);
the return pipe (27) is mounted on the water outlet pipeline at the rear end of the first reversing valve (22) and has a return function;
the rear end of the return pipe (27) is provided with a detection component (28) for detecting;
a second external connecting pipe (29), wherein the top of the detection component (28) is provided with the second external connecting pipe (29);
quick connectors are arranged at the outer side connecting positions of the first external connecting pipe (26) and the second external connecting pipe (29), and the guide-out pump (21), the first reversing valve (22) and the second reversing valve (24) are electrically connected with the controller (6).
2. The apparatus for preparing calcium fluoride powder for nuclei of claim 1, wherein: the air filtering assembly (23) comprises:
the temperature control outer cylinder (231), the top side of the left end of the preparation tank (1) is fixedly provided with the temperature control outer cylinder (231);
the inner side wall of the temperature control outer cylinder (231) is fixedly provided with an adsorption inner cylinder (232) which plays a role in separation and adsorption through bolts;
the outer side wall of the adsorption inner cylinder (232) is fixedly adhered with the heat exchange tube (233) which plays a role in heat exchange;
the water inlets and the water outlets on the upper side and the lower side of the heat exchange tube (233) are connected with the external valve (234) through pipelines;
the baffle (235), the said absorption inner cylinder (232) inboard wall weld has baffles (235) playing a role in churning;
the air outlet pipe (236), the air outlet pipe (236) which plays a role in guiding flow is fixedly welded on the central through hole of the baffle (235);
the quick joint (237) is mounted on the top pipeline of the air outlet pipe (236);
wherein, the inner side wall of the adsorption inner cylinder (232) is provided with a groove which plays a role in flow blocking.
3. The apparatus for preparing calcium fluoride powder for nuclear use according to claim 1, wherein: the dewatering assembly (25) comprises:
the bottom side of the left end of the preparation tank (1) is fixedly provided with a water cylinder (251) with a dewatering function;
the third reversing valve (252) is installed on a water outlet pipeline at the bottom of the dewatering cylinder (251);
wherein the bottom of the third reversing valve (252) is installed with a pipeline at the bottom of the first reversing valve (22) through a connecting pipe;
the fine-pore filter cylinder (253) which plays a role in filtering is rotatably arranged at the bottom of the inside of the dewatering cylinder (251) through a bracket;
the inner side wall of the fine-hole filter cylinder (253) is fixedly adhered with the water filtering cloth (254) which plays a role in filtering;
the toothed ring (255) is mounted on the outer side of the top connecting plate of the fine-hole filter cylinder (253) through bolts and has a transmission function;
the outer side of the gear ring (255) is meshed with the rear end of the transmission gear (256);
the center hole of the transmission gear (256) is connected with a transmission shaft key of the servo motor (257);
the servo motor (257) is installed inside the front side protection box of the dewatering cylinder (251) through bolts, and the third reversing valve (252) and the servo motor (257) are electrically connected with the controller (6).
4. The apparatus for preparing calcium fluoride powder for nuclei of claim 1, wherein: the detection assembly (28) comprises:
the connecting sleeve (281) is arranged on the rear end pipeline of the return pipe (28) and plays a role in flow guiding;
the rear end pipeline of the connecting sleeve (281) is provided with a fourth reversing valve (282) which plays a role in guiding;
the detection barrel (283), the fourth reversing valve (282) is installed at the bottom of the detection barrel (283) through a pipeline;
a fifth reversing valve (284), wherein the top pipeline of the detection barrel (283) is provided with the fifth reversing valve (284) for guiding;
a magnet vibrator (285), wherein the magnet vibrator (285) with the detection function is mounted at the left end of the detection cylinder (283) through a bolt;
a detector (286), wherein the rear end of the detection barrel (283) is mounted with the detector (286) by a bolt;
the sample measuring electrode (287) is fixedly arranged on the upper side of the front end of the detector (286) through a lead;
a reference electrode (288), wherein the reference electrode (288) is fixedly arranged on the lower side of the front end of the detector (286) through a lead;
the fourth reversing valve (282), the fifth reversing valve (284), the magnet vibrator (285), the detector (286), the sample measuring electrode (287) and the reference electrode (288) are all electrically connected with the controller (6).
5. The apparatus for preparing calcium fluoride powder for nuclear use according to claim 1, wherein: the utility model discloses a preparation jar, including preparation jar (1), transmission motor (5) and bolt, preparation jar (1) top middle side bolt is installed and is installed controller (6) at preparation jar (1) front side with the bolt, transmission motor (5) bottom transmission shaft fixed mounting has stirring rake (7) that play the stirring effect, stirring rake (7) are rotated and are set up inside retort (8), preparation jar (1) front end bottom side is equipped with hot water pipe (9).
6. The apparatus for preparing calcium fluoride powder for nuclei of claim 2, wherein: baffle (235) are the heliciform and distribute in the inner wall department that adsorbs inner tube (232), and baffle (235) central through-hole diameter and derive trachea (236).
7. The apparatus for preparing calcium fluoride powder for nuclear use according to claim 3, wherein: the diameters of the filter screens of the fine-pore filter cylinder (253) and the water filtering cloth (254) are respectively 1 cm and 1 mm.
8. The apparatus for preparing calcium fluoride powder for nuclei of claim 3, wherein: the front end of the dewatering cylinder (251) is provided with a connecting box body which plays a role in protecting the servo motor (257).
9. The apparatus for preparing calcium fluoride powder for nuclei of claim 4, wherein: and the top of the fourth reversing valve (282) and the bottom of the fifth reversing valve (284) are respectively provided with a second external connecting pipe (29), and the end heads of the two groups of second external connecting pipes (29) are respectively provided with a quick connector.
10. The method for preparing the calcium fluoride powder for the core according to any one of claims 1 to 9, which is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: quantitatively adding distilled water and ammonium bifluoride raw material: adding a certain amount of distilled water into a reaction tank (8) in a preparation tank (1), introducing external hot water into the preparation tank (1) through a hot water guide pipe (9), heating the distilled water in the reaction tank (8), keeping the distilled water at 60-80 ℃ through controlling the temperature of the external hot water, adding a certain amount of ammonium bifluoride raw material into the reaction tank (8), wherein the solid-liquid ratio of the ammonium bifluoride raw material to the distilled water is 1;
step two: quantitatively and slowly adding calcium carbonate raw materials: then, the calcium carbonate raw material is slowly and quantitatively led into the interior of the reaction tank (8) through the vibration of the discharging bin (3) and is dissolved by stirring, and the ratio of the calcium carbonate raw material to the mixed liquid is 1:7, keeping the interior of the reaction tank (8) at 60-80 ℃ under the action of heat introduced by the hot water guide pipe (9), and fully reacting under the stirring action of the stirring paddle (7), wherein the mixed solution can be introduced into a detection assembly (28) for detection under the driving action of a lead-out pump (21) and a first reversing valve (22);
step three: guiding out filtered gas: then, the mixed liquid in the reaction tank (8) is led out through the lead-out pump (21) and flows into the adsorption inner cylinder (232) under the driving action of the first reversing valve (22), at the moment, the lead-out pump (21) provides lead-out pressure for the liquid, so that the mixed liquid with reaction crystals forms a rotational flow state under the flow blocking action of the baffle (235), and meanwhile, an external refrigerant is led into the heat exchange tube (233) through the external valve (234), so that the heat of the whole adsorption inner cylinder (232) is taken away, the mixed liquid can be contacted with the inner wall of the adsorption inner cylinder (232) under the rotational flow centrifugal action, gas in the mixed liquid can be contacted with the adsorption inner cylinder (232) to be separated from the liquid due to the condensation action of the liquid, so that liquid particles can be attached to the inner side of the adsorption inner cylinder (232), and can be prevented from being taken away by air flow through groove strips on the inner side of the adsorption inner cylinder (232), and separation of hydrogen generated by reaction in the mixed liquid can be improved;
step four: and (3) centrifugal dehydration: then introducing the degassed mixed liquid into the interior of a dewatering component (25) under the action of a second reversing valve (24), collecting the inflowing mixed liquid through a pore filter cartridge (253) and a water filtering cloth (254), controlling a servo motor (257) to drive a transmission gear (256) to rotate through a controller (6) and enabling the transmission gear to be meshed with a toothed ring (255), so that the toothed ring (255) drives the pore filter cartridge (253) and the water filtering cloth (254) to rotate, separating redundant fluorine-containing wastewater from calcium fluoride solids through the filtering effect of the pore filter cartridge (253) and the water filtering cloth (254) and the centrifugal force during rotation, and guiding the redundant fluorine-containing wastewater out through a third reversing valve (252);
step five: and (3) repeated washing: external distilled water is guided into the fine-pore filter cylinder (253) through the flow guiding effect of the second reversing valve (24) and the second external connecting pipe (29) to carry out flushing and washing actions on the calcium fluoride solid;
step six: and (3) detection of the pH value: at the moment, the washing wastewater is led into the first reversing valve (22) due to the reversing effect of the third reversing valve (252), the washing wastewater flows into the detection cylinder (283) through the reversing effect of the first reversing valve (22) and the fourth reversing valve (282), the magnet vibrator (285) is controlled by the controller (6) to oscillate, the sample measuring electrode (287) and the reference electrode (288) are subjected to oscillation waves to generate detection data and transmit the data to the detector (286), and the detector (286) monitors the washing pH value through two sets of data;
step seven: rolling to prepare powder: when the pH value data reaches the standard value, the repeated washing is stopped, and the calcium fluoride solid is taken out for drying and grinding.
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Denomination of invention: Preparation method of nuclear calcium fluoride powder Granted publication date: 20240416 Pledgee: Bank of China Limited by Share Ltd. Shanghai Jingan branch Pledgor: Shanghai Taiyang Technology Co.,Ltd. Registration number: Y2024310000636 |