CN115744827A - Method and device for preparing hydrogen fluoride from fluosilicic acid - Google Patents

Method and device for preparing hydrogen fluoride from fluosilicic acid Download PDF

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Publication number
CN115744827A
CN115744827A CN202211517529.1A CN202211517529A CN115744827A CN 115744827 A CN115744827 A CN 115744827A CN 202211517529 A CN202211517529 A CN 202211517529A CN 115744827 A CN115744827 A CN 115744827A
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fixedly connected
rod
groove
hydrogen fluoride
spring
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CN115744827B (en
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华博文
黄宗发
傅玮兴
廖鸿辉
廖育能
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Fujian Longfu New Material Co ltd
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Fujian Longfu New Material Co ltd
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Abstract

The invention is suitable for the technical field of hydrogen fluoride preparation, and provides a device for preparing hydrogen fluoride from fluosilicic acid, which comprises a reaction kettle, wherein a filter screen is fixedly connected inside the reaction kettle, a flow guide strip is fixedly connected on the inner wall of the reaction kettle, a reciprocating assembly is arranged inside the reaction kettle, a scraping strip for pushing a silica solid to move is arranged on the reciprocating assembly, a reciprocating rod is driven by a chain to move towards one side of a base body inside a reciprocating groove, the reciprocating rod scrapes the silica solid on the filter screen through the scraping strip, the effect of automatically cleaning the residual silica solid is realized, the problem that the filter screen cannot be used due to the fact that the filter screen is blocked by the silica solid is prevented, meanwhile, the silica solid can roll when the silica solid is scraped, the ammonia oxide solution is prevented from remaining on the silica solid, and the problem of waste of the ammonia oxide solution when the silica solid is cleaned can be further prevented.

Description

Method and device for preparing hydrogen fluoride from fluosilicic acid
Technical Field
The invention relates to the technical field of hydrogen fluoride preparation, in particular to a method and a device for preparing hydrogen fluoride from fluosilicic acid.
Background
The hydrogen fluoride is an inorganic compound, the chemical formula is HF, it is colorless under the normal state, the toxic gas that has pungent smell, very strong hygroscopicity has, the contact air produces white smog promptly, easily dissolve in water, can form hydrofluoric acid with water unlimited intersolubility, in-process at hydrogen fluoride preparation, the reactant that its reaction produced has certain retrieval value, can cyclic utilization, current reation kettle can't accomplish automatic the collection to the processing of reactant, and then carry out disposable manual collection after long-time piling up, long-time piling up influences the filter efficiency of filter screen easily, simultaneously because hydrogen fluoride has certain toxicity, if can hardly appear the problem that hydrogen fluoride leaked through artifical manual collection, disposable collection influences certain hydrogen fluoride production process simultaneously, reduce hydrogen fluoride production process linkage, reduce hydrogen fluoride production efficiency.
Therefore, the production device can not automatically collect the available reactant to influence the production efficiency of the hydrogen fluoride.
Therefore, it is necessary to provide a method for preparing hydrogen fluoride by using fluosilicic acid and a device thereof, aiming at solving the problems.
Disclosure of Invention
Aiming at the defects in the prior art, the embodiment of the invention aims to provide a method and a device for preparing hydrogen fluoride by using fluorosilicic acid, and aims to overcome the defect that the production efficiency of the hydrogen fluoride is affected because a production device cannot automatically collect available reactants.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for preparing hydrogen fluoride from fluosilicic acid comprises the following steps:
s1, simultaneously putting fluosilicic acid and ammonia water into a reaction kettle for a two-stage ammoniation reaction to generate an ammonia oxide solution and silicon dioxide, separating the two substances through a filter screen, and collecting the silicon dioxide solids on the filter screen through a collecting mechanism;
s2, enabling the ammonia oxide solution to pass through a filter screen and then react with calcium oxide in the middle of the reaction kettle, generating dilute ammonia water after the ammonia oxide solution reacts, and enabling the dilute ammonia water to enter the top of the reaction kettle again through a backflow mechanism to perform a circulating reaction with fluosilicic acid;
s3, generating calcium fluoride after the calcium oxide reacts, drying ammonia water remaining in the calcium fluoride through a drying mechanism, spraying pure water through a spraying mechanism after drying is finished to perform contact reaction with the calcium fluoride, and further generating hydrogen fluoride and calcium oxide;
s4, recycling the calcium oxide, and reacting the calcium oxide with the ammonia oxide solution again;
and S5, collecting hydrogen fluoride generated in the reaction.
As a further scheme of the invention, the purity of the calcium oxide in the step S2 is more than or equal to 80 percent, and the purity of the calcium oxide secondarily utilized in the step S4 is the same as that of the calcium oxide firstly used.
As a further scheme of the invention, the purity of the ammonia water in the step S1 is the same as that of the dilute ammonia water in the step S2.
The device for preparing hydrogen fluoride from fluosilicic acid comprises a reaction kettle, wherein a filter screen is fixedly connected inside the reaction kettle, a guide strip is fixedly connected on the inner wall of the reaction kettle, a reciprocating component is arranged inside the reaction kettle, a scraping strip used for pushing silica solids to move is arranged on the reciprocating component, a base body is fixedly connected on the outer wall of the reaction kettle, a lifting component is arranged inside the base body, a partition board is vertically and movably connected inside the lifting component, a locking component used for lifting the partition board is arranged at the joint of the lifting component and the partition board, and a processing component used for cleaning the silica solids is arranged at the lower end of the base body.
As a further scheme of the invention, the reciprocating assembly comprises a transmission bin, a reciprocating groove, motors, transmission teeth, a chain, a reciprocating rod, a guide rod, a stabilizing block and a stabilizing rod, the transmission bin is arranged inside the reaction kettle, the reciprocating groove penetrates through the inner wall of the transmission bin, the two motors are fixedly connected inside the transmission bin, the two transmission teeth are fixedly connected to the output ends of the motors, the two ends of the chain are in transmission connection with the transmission teeth, the reciprocating rod is fixedly connected to the chain, the scraping strip is rotatably connected to the reciprocating rod, the guide rod is fixedly connected inside the reaction kettle, the stabilizing block is movably connected to the guide rod, the stabilizing rod is fixedly connected to the upper surface of the scraping strip, and the limit is movably connected to the outer wall of the stabilizing block.
As a further scheme of the invention, the lifting assembly comprises a lifting groove, inclined grooves, a movable opening, a first spring, a movable frame, a first pushing groove, a lifting frame, a second pushing groove and a sliding rod, the lifting groove is formed in the base body, the partition plate is movably connected in the lifting groove, the inner wall of the lifting groove is provided with the two inclined grooves, one end of the first spring is fixedly connected to the inner wall of the reaction kettle, the other end of the first spring is fixedly connected with the outer side end of the movable frame, the outer side end of the movable frame is movably connected to the guide rod, the bottom of the movable frame is movably connected in the movable opening, the first pushing groove is formed in the inner side end of the movable frame, the lifting frame is movably connected in the lifting groove, the outer side end of the lifting frame is movably connected with the two ends of the partition plate in a limiting manner, the second pushing groove penetrates through the lifting frame, the middle of the sliding rod is movably connected in the first pushing groove and the second pushing groove, and the two ends of the sliding rod are movably connected in the inclined grooves.
As a further scheme of the invention, the locking assembly comprises a locking cavity, a stable guide rod, a second spring, a movable rod, a blocking block, a third spring, a second fixture block and a guide strip, the locking cavity is formed in two sides of the partition plate, the stable guide rod is fixedly connected with the inside of the locking cavity, one end of the second spring is fixedly connected with the inner wall of the locking cavity, the other end of the second spring is fixedly connected with the outer wall of the movable rod, the blocking block is fixedly connected with the upper end of the movable rod, one end of the third spring is fixedly connected with the inside of the lifting frame, the other end of the third spring is fixedly connected with the outer side of the second fixture block, and the inner side of the guide strip is mutually clamped with the upper end of the locking cavity.
As a further scheme of the invention, the partition plate further comprises a first clamping block, a clamping groove and an electromagnet, the first clamping block is fixedly connected to the lower end of the movable rod, the guide strip is arranged on the inner side of the base body, two ends of the partition plate are movably connected to the inner side of the guide strip in a limiting manner, the clamping groove is formed in the lower end of the inner side of the guide strip, and the electromagnet is fixedly connected to the outer side of the clamping groove.
As a further aspect of the present invention, the processing assembly includes a heating device, an air drying device, an electric telescopic rod, a movable body, a recycling tank, a fourth spring, a receiving plate, an electric contact and an electric contact tank, the heating device is disposed on the top of the inner wall of the base body, the air drying device is disposed on the top of the inner wall of the base body, the electric telescopic rod is fixedly connected to the bottom of the base body, the outer side of the output end of the electric telescopic rod is fixedly connected to the outer wall of the movable body, the movable body is movably connected to the inside of the base body, the recycling tank is opened inside the base body, the fourth spring is fixedly connected to the recycling tank, the receiving plate is fixedly connected to the top of the fourth spring, the electric contact is fixedly connected to the lower surface of the receiving plate, and the electric contact tank is fixedly connected to the upper surface of the recycling tank.
As a further scheme of the invention, the substrate consists of two parts, namely an inclined pre-storage cavity and a processing cavity for drying the silicon dioxide solids, and grooves for stabilizing are arranged on two sides of the partition plate, so that the partition plate can be stabilized to move up and down.
As a further scheme of the invention, the motor is electrically connected with an external power supply of the equipment, the motor can drive the chain to transmit through the transmission teeth after being electrified, the outer wall of the stabilizing block is symmetrically provided with grooves matched with the stabilizing bars, and the scraping effectiveness of the scraping strips on the silica solids can be stabilized under the sliding action of the stabilizing bars in the grooves on the outer wall of the stabilizing block.
As a further scheme of the invention, the length of the first pushing groove is the same as the height of the chute, the first pushing groove can effectively drive the sliding rod to slide up and down in the chute, the length of the second pushing groove is matched with the left and right intervals of the chute, and the sliding rod can effectively drive the lifting frame to move up and down through the second pushing groove.
As a further scheme of the invention, the upper end and the lower end of the locking cavity penetrate through the outside to facilitate the outward movement of the blocking block and the first fixture block, the first fixture block is made of magnetic conductive material and can be magnetically attracted by the electromagnet, the inner side end of the second fixture block is made into a spherical shape to facilitate the blocking block to push the second fixture block to be incapable of being clamped with the upper end of the locking cavity, the electromagnet is electrically connected with the electrical contact, and the electromagnet can generate magnetic force to magnetically attract the first fixture block after being electrified.
As a further scheme of the invention, the electric telescopic rod is electrically connected through an external timing control device, so that the electric telescopic rod can be controlled to shrink in a timing mode after an electric contact is electrically contacted with an electric contact groove, the movable body is arranged to be hollow on one side and solid on the other side, when the movable body moves outwards in a hollow mode, a solid part of the movable body can seal the inside of the base body, the air drying device and the electric contact groove are electrically connected with an external power supply, the heating device can heat and dry silicon dioxide after being electrified, and the air drying device can perform the air drying function on the silicon dioxide by matching with heat of the heating device after being electrified.
Compared with the prior art, the method and the device for preparing hydrogen fluoride from fluosilicic acid have the beneficial effects that:
1. the device for preparing hydrogen fluoride from fluosilicic acid can drive the reciprocating rod to move to one side of the base body in the reciprocating groove through the chain, the reciprocating rod scrapes silica solids on the filter screen through the scraping strip, the effect of automatically cleaning the residual silica solids is achieved, the problem that the filter screen cannot be used due to the fact that the silica solids block the filter screen is solved, meanwhile, the silica solids can roll when the silica solids are scraped, ammonia oxide solution is prevented from remaining on the silica solids, and the problem that the ammonia oxide solution is wasted when the silica solids are cleaned can be solved;
2. the device for preparing hydrogen fluoride from fluosilicic acid can ensure the stability of the scraping strip in the movement process under the limiting action of the stabilizing rod on the outer wall of the stabilizing block, prevent the problem that the silicon dioxide solids cannot be scraped due to the looseness of the scraping strip when the silicon dioxide solids are scraped, and improve the effectiveness of the scraping strip in scraping the silicon dioxide solids;
3. according to the device for preparing hydrogen fluoride from fluosilicic acid, after the heating device and the air drying device are electrified, the heating device heats the silica solids, and meanwhile, the air drying device blows hot gas to air the silica solids, so that residual ammonia oxide solution is prevented from flowing out when the silica solids are collected, and the safety of the device in use is improved;
4. the device for preparing hydrogen fluoride from fluosilicic acid can drive the partition plate to move downwards through the second fixture block by the lifting frame, so that the base body is cut again, the base body can be further cut into a pre-storage cavity and a treatment cavity, hot gas of the heating device in the heating process can be prevented from being diffused and entering the inside of the reaction kettle, the influence of the hot gas on the internal reaction of the reaction kettle is reduced, and the stability of the internal reaction of the reaction kettle is ensured;
5. according to the device for preparing hydrogen fluoride from fluosilicic acid, the movable body can be driven to move to the other side through the electric telescopic rod, the movable body pushes the dried silicon dioxide solid on the bearing plate to move outwards, and the silicon dioxide solid is collected through the external collecting device, so that the automatic collecting effect is realized, the manual collecting steps are effectively reduced, the collecting efficiency of reaction residues is improved, and meanwhile, the secondary utilization effect can be quickly realized.
To more clearly illustrate the structural features and effects of the present invention, the present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
Drawings
FIG. 1 is a perspective view of the overall structure of the present invention;
FIG. 2 is a schematic partial perspective view of the internal structure of the base body according to the present invention;
FIG. 3 is a perspective view of the inner structure of the reciprocating groove of the present invention;
FIG. 4 is a perspective view of the internal structure of the reciprocating assembly of the present invention;
FIG. 5 is a sectional partial perspective view of a scraper strip according to the present invention;
FIG. 6 is an enlarged view of the structure at A in FIG. 5 according to the present invention;
FIG. 7 is a perspective view of the internal structure of the lift assembly of the present invention;
FIG. 8 is an enlarged view of the structure at B in FIG. 7 according to the present invention;
FIG. 9 is a schematic top partial perspective view of the internal structure of the lifting slot of the present invention;
FIG. 10 is an enlarged view of the structure at C of FIG. 9 according to the present invention;
FIG. 11 is a partial perspective view of the inner structure of the locking assembly of the present invention;
FIG. 12 is an enlarged view of the structure of FIG. 11 at D in accordance with the present invention;
fig. 13 is a perspective view of the movable body structure according to the present invention.
Reference numerals: 1. a reaction kettle; 2. filtering with a screen; 3. a flow guide strip;
4. a reciprocating assembly; 401. a transmission bin; 402. a reciprocating groove; 403. a motor; 404. a transmission gear; 405. a chain; 406. a reciprocating lever; 407. a guide bar; 408. a stabilizing block; 409. a stabilizer bar;
5. scraping the strip; 6. a base;
7. a lifting assembly; 701. a lifting groove; 702. a chute; 703. a movable opening; 704. a first spring; 705. a movable frame; 706. a first push slot; 707. a lifting frame; 708. a second push groove; 709. a slide bar;
8. a partition plate;
9. a locking assembly; 901. a lock cavity; 902. stabilizing the guide rod; 903. a second spring; 904. a movable rod; 905. a plugging block; 906. a first clamping block; 907. a third spring; 908. a second fixture block; 909. a guide strip; 910. a card slot; 911. an electromagnet;
10. a processing component; 1001. a heating device; 1002. an air drying device; 1003. an electric telescopic rod; 1004. a movable body; 1005. a recovery tank; 1006. a fourth spring; 1007. a bearing plate; 1008. an electrical contact; 1009. and electrically contacting the groove.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
In the description of the present invention, the terms "central," "lateral," "upper," "lower," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in an orientation or positional relationship indicated based on the orientation or positional relationship shown in the drawings, merely for convenience in describing the invention and for simplicity in description, and are not intended to indicate or imply that the device or element so referred to must have a particular orientation, be constructed in a particular orientation, and be operated in a particular manner, and therefore, are not to be construed as limiting the invention.
Specific implementations of the present invention are described in detail below with reference to specific embodiments.
Example one
As a preferred embodiment of the present invention, a method for preparing hydrogen fluoride from fluosilicic acid comprises:
s1, simultaneously putting fluosilicic acid and ammonia water into a reaction kettle 1 for a two-stage ammoniation reaction to generate an ammonia oxide solution and silicon dioxide, separating the two substances through a filter screen 2, and collecting the silicon dioxide solids on the filter screen 2 through a collecting mechanism;
s2, enabling the ammonia oxide solution to pass through the filter screen 2 and then react with calcium oxide in the middle of the reaction kettle, generating dilute ammonia water after the ammonia oxide solution reacts, and enabling the dilute ammonia water to enter the top of the reaction kettle again through a backflow mechanism to perform a circulating reaction with fluosilicic acid;
s3, generating calcium fluoride after the calcium oxide reacts, drying ammonia water remaining in the calcium fluoride through a drying mechanism, spraying pure water through a spraying mechanism after drying is finished to perform contact reaction with the calcium fluoride, and further generating hydrogen fluoride and calcium oxide;
s4, recycling the calcium oxide, and reacting the calcium oxide with the ammonia oxide solution again;
and S5, collecting hydrogen fluoride generated in the reaction.
As a further scheme of the invention, the purity of the calcium oxide in the step S2 is more than or equal to 80 percent, and the purity of the calcium oxide secondarily utilized in the step S4 is the same as that of the calcium oxide firstly used.
As a further scheme of the invention, the purity of the ammonia water in the step S1 is the same as that of the dilute ammonia water in the step S2.
Example two
As shown in fig. 1 to 13, as a preferred embodiment of the present invention, an apparatus for preparing hydrogen fluoride from fluorosilicic acid comprises a reaction vessel 1, a filter screen 2 is fixedly connected inside the reaction vessel 1, a flow guide strip 3 is fixedly connected to an inner wall of the reaction vessel 1, a reciprocating assembly 4 is arranged inside the reaction vessel 1, a scraping strip 5 for pushing a silica solid to move is arranged on the reciprocating assembly 4, a base body 6 is fixedly connected to an outer wall of the reaction vessel 1, the base body 6 is composed of two parts, namely an inclined pre-storage cavity and a silica solid drying treatment cavity, a lifting assembly 7 is arranged inside the base body 6, a partition plate 8 is vertically and movably connected inside the lifting assembly 7, grooves for stabilizing the partition plate 8 are arranged on two sides of the partition plate 8, an up-and-down movement of the partition plate 8 can be stabilized, a locking assembly 9 for fixing the lifting of the partition plate 8 is arranged at a connection position of the lifting assembly 7 and the partition plate 8, and a treatment assembly 10 for cleaning the silica solid.
Preferably, in this embodiment, during the use, through fluosilicic acid with aqueous ammonia after the inside reaction of reation kettle 1 produce oxidation ammonia solution and silica solid, after the separation through filter screen 2, oxidation ammonia solution continues to react downwards after passing through filter screen 2, silica is piled up on filter screen 2, drive through reciprocal subassembly 4 and scrape strip 5 reciprocating motion, and then scrape silica solid to the inside of base member 6 on filter screen 2 through scraping strip 5 ceaselessly, when reciprocal subassembly 4 scrapes silica solid through scraping strip 5 and moves the one side that is close to base member 6 on filter screen 2, reciprocal subassembly 4 makes lift assembly 7 drive baffle 8 upward movement through locking subassembly 9, the silica solid drops on processing assembly 10 under the effect of the prestorage chamber of base member 6 slope, dry the silica solid through processing assembly 10, the realization is to remaining oxidation ammonia solution on preventing the silica solid, when placing too much silica on processing assembly 10, locking subassembly 9 contact and lift assembly 7 and baffle 8's joint relation this moment, make baffle 8 joint in the position through locking subassembly 9, baffle 8 is carrying out the processing assembly 6 when the silica solid that the processing assembly 10 gets into the external connection of the processing assembly 10 of silica solid and collection, the heat of the processing assembly after the silica solid makes the whole processes the silica solid of silica collection, it push out the processing assembly to utilize the external solid to carry out the processing assembly to carry out the processing at regular time.
EXAMPLE III
As shown in fig. 1 to 10, as a preferred embodiment of the present invention, the reciprocating assembly 4 includes a transmission bin 401, a reciprocating groove 402, a motor 403, transmission teeth 404, a chain 405, a reciprocating rod 406, a guide rod 407, a stabilizing block 408 and a stabilizing rod 409, the transmission bin 401 is disposed inside the reaction kettle 1, the reciprocating groove 402 penetrates through the inner wall of the transmission bin 401, the two motors 403 are both fixedly connected inside the transmission bin 401, the motors 403 are electrically connected to an external power source of the apparatus, the motors 403 can drive the chain 405 to perform transmission through the transmission teeth 404 after being powered on, the two transmission teeth 404 are both fixedly connected to the output end of the motors 403, both ends of the chain 405 are both in transmission connection with the transmission teeth 404, the reciprocating rod 406 is fixedly connected to the stabilizing rod 405, the scraping bar 5 is rotatably connected to the reciprocating rod 406, the guide rod 407 is fixedly connected inside the reaction kettle 1, the stabilizing block 408 is movably connected to the guide rod 407, grooves adapted to the outer wall of the stabilizing block 408 are symmetrically formed on the outer wall of the stabilizing rod 408, the stabilizing rod 409 can be stably connected to the outer wall of the scraping bar 5 under the sliding action inside the stabilizing rod 408, and the outer wall of the stabilizing rod 408 is movably connected to the upper surface of the silica scraping surface of the stabilizing block 409.
The lifting component 7 comprises a lifting groove 701, inclined grooves 702, a movable port 703, a first spring 704, a movable frame 705, a first pushing groove 706, a lifting frame 707, a second pushing groove 708 and a sliding rod 709, the lifting groove 701 is arranged in the base 6, a partition plate 8 is movably connected in the lifting groove 701, the inner wall of the lifting groove 701 is provided with two inclined grooves 702, one end of the first spring 704 is fixedly connected with the inner wall of the reaction kettle 1, the other end of the first spring 704 is fixedly connected with the outer side end of the movable frame 705, the outer side end of the movable frame 705 is movably connected with a guide rod 407, the bottom of the movable frame 705 is movably connected in the movable port 703, the first pushing groove 706 is arranged at the inner side end of the movable frame 705, the length of first promotion groove 706 is the same with chute 702's height, first promotion groove 706 can be effectual drives slide bar 709 and slides from top to bottom in chute 702's inside, crane 707 swing joint is in the inside of lifting groove 701, the outside end of crane 707 and the spacing swing joint in both ends of baffle 8, second promotes groove 708 and runs through and sets up on crane 707, the length of second promotes groove 708 and the left and right sides interval looks adaptation of chute 702, slide bar 709 can be effectual drives crane 707 up-and-down motion through second promotion groove 708, the middle part swing joint of slide bar 709 is in the inside of first promotion groove 706 and second promotion groove 708, the both ends swing joint of slide bar 709 is in chute 702's inside.
Example four
As shown in fig. 1, 2, 4, 7, 11, 12 and 13, as a preferred embodiment of the present invention, the locking assembly 9 includes a locking cavity 901, a stable guide rod 902, a second spring 903, a movable rod 904, a blocking block 905, a third spring 907, a second blocking block 908 and a guide strip 909, the locking cavity 901 is opened at two sides of the partition plate 8, both upper and lower ends of the locking cavity 901 penetrate through the outside to facilitate the outward movement of the blocking block 905 and the first blocking block 906, the stable guide rod 902 is fixedly connected to the inside of the locking cavity 901, one end of the second spring 903 is fixedly connected to the inner wall of the locking cavity 901, the other end of the second spring 903 is fixedly connected to the outer wall of the movable rod 904, the blocking block 905 is fixedly connected to the upper end of the movable rod 904, one end of the third spring 907 is fixedly connected to the inside of the lifting frame 707, the other end of the third spring 907 is fixedly connected to the outside of the second blocking block 908, the inner end of the second blocking block 908 is spherical, so that the blocking block 905 pushes the second blocking block 908 to be clamped to the upper end of the locking cavity and the upper end of the guide strip 901, and the guide strip 901 are clamped to each other.
The partition plate 8 further comprises a first fixture block 906, a clamping groove 910 and an electromagnet 911, the first fixture block 906 is fixedly connected to the lower end of the movable rod 904, the first fixture block 906 is made of magnetic conductive materials and can be magnetically attracted by the electromagnet 911, the guide strip 909 is arranged on the inner side of the base body 6, the two ends of the partition plate 8 are movably connected to the inner side of the guide strip 909 in a limiting mode, the clamping groove 910 is formed in the lower end of the inner side of the guide strip 909, the electromagnet 911 is fixedly connected to the outer side of the clamping groove 910, the electromagnet 911 is electrically connected with the electric contact 1008, and the electromagnet 911 can generate magnetic attraction to attract the first fixture block 906 after being electrified.
The treatment component 10 comprises a heating device 1001, an air drying device 1002, an electric telescopic rod 1003, a movable body 1004, a recovery tank 1005, a fourth spring 1006, a bearing plate 1007, an electric contact 1008 and an electric contact groove 1009, wherein the heating device 1001 is arranged on the top of the inner wall of the base body 6, the heating device 1001 is electrically connected with an external power supply, the heating device 1001 can heat and dry silicon dioxide after being electrified, the air drying device 1002 is arranged on the top of the inner wall of the base body 6, the air drying device 1002 is electrically connected with the external power supply, the electric telescopic rod 1003 is fixedly connected to the bottom of the base body 6 after the air drying device 1002 is electrified and is matched with the heat of the heating device 1001 to perform air drying on the silicon dioxide, the outer side of the output end of the electric telescopic rod 1003 is fixedly connected with the outer wall of the movable body 1004, electric telescopic handle 1003 is through external timing control device electric connection, play and to control the effect that electric telescopic handle 1003 contracts regularly after electric contact 1008 and electric contact groove 1009 electric contact, activity body 1004 swing joint is in the inside of base member 6, it is solid that activity body 1004 sets up to the hollow opposite side in one side, its solid partly can carry out the shutoff to the inside of base member 6 when activity body 1004 hollow outside motion, accumulator 1005 sets up in the inside of base member 6, fourth spring 1006 fixed connection is on accumulator 1005, accept board 1007 fixed connection at the top of fourth spring 1006, electric contact 1008 fixed connection is on the lower surface of accepting board 1007, electric contact groove 1009 fixed connection is on the upper surface of accumulator 1005, electric contact groove 1009 and external power supply electric connection.
The overall working principle of the first to fourth embodiments is as follows:
in an initial state, the fourth spring 1006 is in a relaxed and extended state, the receiving plate 1007 is in a highest position by the fourth spring 1006, the receiving plate 1007 and the hollow position of the movable body 1004 are clamped with each other, the electric contact 1008 is not in electric contact with the electric contact groove 1009, the electric contact 1008 is in a power-off state, at this time, the electromagnet 911 is in a power-off and non-magnetic state, the second spring 903 is in a contracted state, the movable rod 904 is in an innermost side of the locking cavity 901 by the second spring 903, the third spring 907 is in a relaxed and extended state, the second fixture block 908 is clamped with the upper end of the locking cavity 901 by the third spring 907, the outer side of the movable frame 705 is not extruded, the first spring 704 is in a relaxed and extended state, the movable frame 705 is in an outermost side, the movable frame 705 drives the sliding rod 709 to be in a lowest position of the chute 702 through the first pushing groove 706, the lifting frame 709 drives the lifting frame 707 to be in a lowest position through the second fixture block 708, and further divides the base 6.
When in work, the fluosilicic acid and the ammonia water react in the reaction kettle 1 to generate an ammonia oxide solution and a silicon dioxide solid, after the ammonia oxide solution is separated by the filter screen 2, the ammonia oxide solution continuously reacts downwards through the filter screen 2, the silicon dioxide is accumulated on the filter screen 2, because the motor 403 is electrically connected to an external power source of the device, when the motor 403 is controlled to be powered on, the motor 403 drives the transmission gear 404 fixed on the output end to rotate counterclockwise, the transmission gear 404 drives the chain 405 to perform counterclockwise transmission, the chain 405 drives the reciprocating rod 406 to reciprocate counterclockwise in the reciprocating groove 402, because the transmission of the chain 405 has a height difference, when the chain 405 drives the reciprocating rod 406 to move to the bottom position of the reciprocating groove 402, the reciprocating rod 406 drives the stabilizing rod 409 to move downwards on the outer wall of the stabilizing block 408 through the scraping strip 5, under the action of the limiting movement of the stabilizing rod 409 on the outer wall of the stabilizing block 408, the stability of the scraping strip 5 in the movement process can be ensured, the problem that the silicon dioxide solid cannot be scraped due to the looseness of the scraping strip 5 when the silicon dioxide solid is scraped is prevented, the effectiveness of scraping the silicon dioxide solid by the scraping strip 5 is improved, when the reciprocating rod 406 is driven by the chain 405 to move towards one side of the base body 6 in the reciprocating groove 402, the reciprocating rod 406 can scrape the silica solids on the filter screen 2 through the scraping strip 5, so as to realize the effect of automatically cleaning the residual silica solids, prevent the problem that the filter screen 2 cannot be used due to the blockage of the filter screen 2 by the silica solids, meanwhile, when the silicon dioxide solid is scraped, the silicon dioxide solid can roll, the ammonia oxide solution is prevented from remaining on the silicon dioxide solid, and then the problem of waste of the ammonia oxide solution can be prevented when the silica solids are cleaned.
When the silica solids are scraped to one side close to the base body 6 by the scraping strip 5, the scraping strip 5 drives the stabilizing block 408 to move to one side of the base body 6 on the guide rod 407 through the stabilizing rod 409, after the stabilizing block 408 abuts against the outer side end of the movable frame 705, the stabilizing block 408 pushes the movable frame 705 to move towards the inside of the lifting groove 701 through the movable port 703 and compress the first spring 704, the movable frame 705 drives the sliding rod 709 to slide upwards in the chute 702 through the first pushing groove 706, the sliding rod 709 enables the lifting frame 707 to move upwards through the second pushing groove 708, the lifting frame 707 drives the partition plate 8 to move upwards in the lifting groove 701 through the second fixture block 908, because the side of the base body 6 close to the reaction kettle 1 is provided with the inclined pre-storage cavity, the stabilizing rod rolls downwards to the bearing plate 1007 under the action of the inclined pre-storage cavity, because the heating device 1001 and the air drying device 1002 are both electrically connected with the external power supply, after the heating device 1001 is electrified, the heating device 1001 heats the silica solids, and the air drying device 1002 blows the silica solids, when the silica solids to move towards the side of the base body 6, the stabilizing rod 408, the side of the base body 405 is far away from the stabilizing rod 408, when the reciprocating rod 408, the stabilizing rod 408, the ammonia collecting device 408 moves towards the side of the base body 405, the stabilizing rod 408, the stabilizing block 408, when the ammonia solution is moved towards the side of the base body 405, the stabilizing rod 408, the ammonia collecting device 405 moves towards the base body 405, the stabilizing rod 408, the ammonia collecting device 405 moves upwards, the stabilizing block 408 cannot extrude the movable frame 705, the movable frame 705 moves to the outer side of the lifting groove 701 under the action of the extension of the first spring 704, the movable frame 705 drives the sliding rod 709 to move downwards in the chute 702 through the first pushing groove 706, the sliding rod 709 drives the lifting frame 707 to move downwards through the second pushing groove 708, the lifting frame 707 drives the partition plate 8 to move downwards through the second fixture block 908, the base body 6 is further divided into a pre-storage cavity and a treatment cavity, the hot gas emission of the heating device 1001 in the heating process can be prevented from entering the inside of the reaction kettle 1, the influence of the hot gas on the internal reaction of the reaction kettle 1 is further reduced, and the stability of the internal reaction of the reaction kettle 1 is ensured.
When the weight of the silica solid on the bearing plate 1007 is greater than the elastic force of the fourth spring 1006, the silica solid makes the bearing plate 1007 move downward into the recycling tank 1005 and compress the fourth spring 1006, the bearing plate 1007 cannot be clamped with the hollow position of the movable body 1004, the bearing plate 1007 drives the electrical contact 1008 to electrically contact with the electrical contact 1009, because the electrical contact 1009 is electrically connected with the external power supply of the device, the electrical contact 1009 energizes the electrical contact 1008, because the electrical contact 1008 is electrically connected with the electromagnet 911, the electromagnet 911 is energized, magnetism is generated after the electromagnet 911 is energized, when the partition plate 8 moves downward to the lowest position, the partition plate 8 drives the first fixture block 906 to horizontally coincide with the fixture groove 910, because the first fixture block 906 is made of a magnetic conductive material, and the first fixture block 906 drives the movable rod 904 to move outward in the locking cavity 901 under the action of the magnetic attraction force 911 of the electromagnet, the first fixture block 906 moves outwards to the inside of the clamping groove 910 for clamping, the movable rod 904 moves outwards stably through the stabilizing guide rod 902 and stretches the second spring 903 in the process of moving outwards, the movable rod 904 drives the blocking block 905 to move outwards, the blocking block 905 extrudes the second fixture block 908 clamped at the upper end of the locking cavity 901, the second fixture block 908 moves towards the inside of the lifting frame 707 and compresses the third spring 907, at the moment, the second fixture block 908 cannot be clamped with the upper end of the locking cavity 901, the connection between the lifting assembly 7 and the partition plate 8 is released, the lifting assembly 7 cannot drive the partition plate 8 to move upwards and downwards, the partition plate 8 is locked at the lowest position, the base body 6 is effectively fixedly divided, further, silica solid objects are prevented from continuously falling onto the bearing plate 1007, and the silica solid objects can be stored temporarily through the inclined pre-storage cavity, heating device 1001 dries with air-dry device 1002 to accepting silica solids on board 1007 continuously this moment, after drying a period, through the shrink of external timing control device control electric telescopic handle 1003, electric telescopic handle 1003 drives activity body 1004 and moves to the opposite side, activity body 1004 promotes and accepts silica solids after drying on board 1007 and moves to the outside, collect through external collection device this moment, the effect of automatic collection has been realized, the effectual step of manual collection that has reduced, the collection efficiency of reaction residue is improved, also can carry out the effect of reutilization fast simultaneously.
It should be noted that all the components in the present application are general standard components or components known to those skilled in the art, which effectively solve the problem that the production efficiency of hydrogen fluoride is affected because the production device cannot be automated to collect the available reactants.
Although several embodiments and examples of the present invention have been described for those skilled in the art, these embodiments and examples are presented as examples and are not intended to limit the scope of the invention. These new embodiments can be implemented in other various ways, and various omissions, substitutions, and changes can be made without departing from the spirit of the invention. These embodiments and modifications thereof are included in the scope and gist of the invention, and are included in the invention described in the claims and the equivalent scope thereof.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (9)

1. A method for preparing hydrogen fluoride from fluosilicic acid is characterized by comprising the following steps:
s1, simultaneously putting fluosilicic acid and ammonia water into a reaction kettle for a two-stage ammoniation reaction to generate an ammonia oxide solution and silicon dioxide, separating the two substances through a filter screen, and collecting the silicon dioxide solid retained on the filter screen through a collecting mechanism;
s2, enabling the ammonia oxide solution to pass through a filter screen and then react with calcium oxide in the middle of the reaction kettle, generating dilute ammonia water after the ammonia oxide solution reacts, and enabling the dilute ammonia water to enter the top of the reaction kettle again through a backflow mechanism to perform a circulating reaction with fluosilicic acid;
s3, calcium fluoride is generated after the calcium oxide reacts, ammonia water remaining in the calcium fluoride is dried through a drying mechanism, and after drying is finished, a spraying mechanism is used for spraying pure water to perform contact reaction with the calcium fluoride, so that hydrogen fluoride and calcium oxide are generated;
s4, recycling the calcium oxide, and reacting the calcium oxide with the ammonia oxide solution again;
and S5, collecting hydrogen fluoride generated by the reaction.
2. The method for preparing hydrogen fluoride by using fluosilicic acid as claimed in claim 1, wherein the purity of the calcium oxide in step S2 is 80% or more, and the purity of the calcium oxide reused in step S4 is the same as the purity of the calcium oxide used for the first time.
3. The method for preparing hydrogen fluoride by using fluosilicic acid as claimed in claim 1, wherein the purity of the ammonia water in step S1 is the same as that of the dilute ammonia water in step S2.
4. An apparatus for preparing hydrogen fluoride from fluorosilicic acid, which is applied to the method for preparing hydrogen fluoride from fluorosilicic acid as defined in any one of claims 1 to 3, and which comprises a reaction kettle (1), wherein a filter screen (2) is fixedly connected to the inside of the reaction kettle (1), a flow guide strip (3) is fixedly connected to the inner wall of the reaction kettle (1), a reciprocating assembly (4) is arranged inside the reaction kettle (1), a scraping strip (5) for pushing silica solids to move is arranged on the reciprocating assembly (4), a base body (6) is fixedly connected to the outer wall of the reaction kettle (1), a lifting assembly (7) is arranged inside the base body (6), a partition plate (8) is vertically movably connected to the inside of the lifting assembly (7), a locking assembly (9) for fixing the partition plate (8) to lift is arranged at the connection position of the lifting assembly (7) and the partition plate (8), and a treatment assembly (10) for cleaning the silica solids is arranged at the lower end of the base body (6).
5. The device for preparing hydrogen fluoride from fluosilicic acid according to claim 4, wherein the reciprocating assembly (4) comprises a transmission bin (401), a reciprocating groove (402), a motor (403), transmission teeth (404), a chain (405), a reciprocating rod (406), a guide rod (407), a stabilizing block (408) and a stabilizing rod (409), the transmission bin (401) is arranged in the reaction kettle (1), the reciprocating groove (402) is arranged on the inner wall of the transmission bin (401) in a penetrating manner, the two motors (403) are fixedly connected in the transmission bin (401), the two transmission teeth (404) are fixedly connected at the output end of the motors (403), the two ends of the chain (405) are connected with the transmission teeth (404) in a driving manner, the reciprocating rod (406) is fixedly connected on the chain (405), the scraping strip (5) is rotatably connected on the reciprocating rod (406), the guide rod (407) is fixedly connected in the reaction kettle (1), the stabilizing rod (408) is movably connected on the guide rod (408), the outer wall of the stabilizing rod (407) is fixedly connected on the scraping surface (409), and the stabilizing rod (409) is movably connected on the upper surface of the stabilizing rod (408).
6. The device for preparing hydrogen fluoride from fluosilicic acid according to claim 5, wherein the lifting assembly (7) comprises a lifting groove (701), a chute (702), a movable port (703), a first spring (704), a movable frame (705), a first pushing groove (706), a lifting frame (707), a second pushing groove (708) and a sliding rod (709), the lifting groove (701) is arranged inside the base body (6), the partition plate (8) is movably connected inside the lifting groove (701), the inner wall of the lifting groove (701) is provided with two chutes (702), the movable port (703) is arranged on the reaction vessel (1) in a penetrating manner, the movable port (703) and the lifting groove (701) are communicated with each other, one end of the first spring (704) is fixedly connected to the inner wall of the reaction vessel (1), the other end of the first spring (704) is fixedly connected to the outer end of the movable frame (705), the outer end of the movable frame (705) is movably connected to a guide rod (407), the bottom of the movable frame (705) is movably connected to the inner end of the movable frame (703), the lifting frame (707) is connected to the inner side end of the lifting groove (707), the inner wall (707) is connected to the lifting groove (707), the inner end of the lifting groove (1) is connected to the lifting groove (1), the second pushing groove (708) penetrates through the lifting frame (707), the middle part of the sliding rod (709) is movably connected to the inside of the first pushing groove (706) and the second pushing groove (708), and two ends of the sliding rod (709) are movably connected to the inside of the chute (702).
7. The device for preparing hydrogen fluoride by using fluosilicic acid as claimed in claim 6, wherein the locking assembly (9) comprises a locking cavity (901), a stable guide rod (902), a second spring (903), a movable rod (904), a blocking block (905), a third spring (907), a second clamping block (908) and a guide strip (909), the locking cavity (901) is arranged on two sides of the partition plate (8), the stable guide rod (902) is fixedly connected with the inside of the locking cavity (901), one end of the second spring (903) is fixedly connected with the inner wall of the locking cavity (901), the other end of the second spring (903) is fixedly connected with the outer wall of the movable rod (904), the blocking block (905) is fixedly connected with the upper end of the movable rod (904), one end of the third spring (907) is fixedly connected with the inside of the lifting frame (707), the other end of the third spring (907) is fixedly connected with the outer side of the second clamping block (908), and the inner side of the guide strip (909) is mutually clamped with the upper end of the locking cavity (901).
8. The device for preparing hydrogen fluoride by using fluosilicic acid according to claim 7, wherein the partition plate (8) further comprises a first clamping block (906), a clamping groove (910) and an electromagnet (911), the first clamping block (906) is fixedly connected to the lower end of the movable rod (904), the guide strip (909) is arranged on the inner side of the base body (6), the two ends of the partition plate (8) are movably connected to the inner side of the guide strip (909) in a limiting manner, the clamping groove (910) is arranged at the lower end of the inner side of the guide strip (909), and the electromagnet (911) is fixedly connected to the outer side of the clamping groove (910).
9. The device for preparing hydrogen fluoride from fluosilicic acid according to claim 4, wherein the processing assembly (10) comprises a heating device (1001), an air drying device (1002), an electric telescopic rod (1003), a movable body (1004), a recovery tank (1005), a fourth spring (1006), a receiving plate (1007), an electric contact (1008) and an electric contact tank (1009), the heating device (1001) is arranged on the top of the inner wall of the base body (6), the air drying device (1002) is arranged on the top of the inner wall of the base body (6), the electric telescopic rod (1003) is fixedly connected to the bottom of the base body (6), the outer side of the output end of the electric telescopic rod (1001) is fixedly connected to the outer wall of the movable body (1004), the movable body (1004) is movably connected to the inside of the base body (6), the recovery tank (1005) is arranged inside the base body (6), the fourth spring (1006) is fixedly connected to the recovery tank (1005), the receiving plate (1007) is fixedly connected to the top of the fourth spring (1006), the electric contact (1008) is fixedly connected to the lower surface of the receiving plate (1005), and the upper surface of the recovery tank (1003) is fixedly connected to the upper surface of the recovery tank (1005).
CN202211517529.1A 2022-11-30 2022-11-30 Method and device for preparing hydrogen fluoride from fluosilicic acid Active CN115744827B (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1236716A (en) * 1968-12-20 1971-06-23 Alfa Laval Ab Transmission system for mechanical stable cleaner
CN105645358A (en) * 2016-03-14 2016-06-08 衢州市鼎盛化工科技有限公司 Method for preparing hydrogen fluoride from fluosilicic acid
CL2015003095A1 (en) * 2015-10-20 2016-07-01 Picozzi Augusto Reijer Sludge dehydrator
CN107055477A (en) * 2017-04-26 2017-08-18 衢州市鼎盛化工科技有限公司 The method and its device of hydrogen fluoride are prepared by fluosilicic acid
CN210473156U (en) * 2019-07-30 2020-05-08 徐州徐工环境技术有限公司 Sewage and sludge treatment device with reciprocating scraper mechanism
CN214130499U (en) * 2020-12-12 2021-09-07 江西飞宇新能源科技有限公司 A cleaning device for production of battery level lithium carbonate
WO2022120967A1 (en) * 2020-12-09 2022-06-16 淄博创立机电科技有限公司 Multi-anti-clogging-type wastewater treatment device
CN114639886A (en) * 2022-03-14 2022-06-17 太和县大华能源科技有限公司 Environment-friendly high-recovery-rate waste storage battery recovery processing method

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1236716A (en) * 1968-12-20 1971-06-23 Alfa Laval Ab Transmission system for mechanical stable cleaner
CL2015003095A1 (en) * 2015-10-20 2016-07-01 Picozzi Augusto Reijer Sludge dehydrator
CN105645358A (en) * 2016-03-14 2016-06-08 衢州市鼎盛化工科技有限公司 Method for preparing hydrogen fluoride from fluosilicic acid
CN107055477A (en) * 2017-04-26 2017-08-18 衢州市鼎盛化工科技有限公司 The method and its device of hydrogen fluoride are prepared by fluosilicic acid
CN210473156U (en) * 2019-07-30 2020-05-08 徐州徐工环境技术有限公司 Sewage and sludge treatment device with reciprocating scraper mechanism
WO2022120967A1 (en) * 2020-12-09 2022-06-16 淄博创立机电科技有限公司 Multi-anti-clogging-type wastewater treatment device
CN214130499U (en) * 2020-12-12 2021-09-07 江西飞宇新能源科技有限公司 A cleaning device for production of battery level lithium carbonate
CN114639886A (en) * 2022-03-14 2022-06-17 太和县大华能源科技有限公司 Environment-friendly high-recovery-rate waste storage battery recovery processing method

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