CN108658081A - The method and its production equipment of ocratation are produced using prodan as raw material - Google Patents
The method and its production equipment of ocratation are produced using prodan as raw material Download PDFInfo
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- CN108658081A CN108658081A CN201810867476.3A CN201810867476A CN108658081A CN 108658081 A CN108658081 A CN 108658081A CN 201810867476 A CN201810867476 A CN 201810867476A CN 108658081 A CN108658081 A CN 108658081A
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- prodan
- ocratation
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- nitrogen
- groove body
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/10705—Tetrafluoride
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The present invention relates to a kind of methods and its production equipment producing ocratation using prodan as raw material, it mainly produces hydrogen fluoride with sulfuric acid reaction by prodan and needs ocratation to be prepared, and the hydrogen fluoride gas of generation various recycle, integrate so that hydrogen fluoride further reflects ocratation with silicon dioxde reaction；Beneficial effects of the present invention：Production cost is low, production efficiency is high, yield is high.
Description
Technical field
It is the present invention relates to ocratation production technical field, more particularly to a kind of using prodan as raw material production four
The method and its production equipment of silicon fluoride.
Background technology
Ocratation refers to a kind of colourless, toxic smell excitatory, is mainly used for cement and artificial marble
The synthetic material of curing agent and organo-silicon compound；In the prior art, generally use hydrofluoric acid (HFH2O) and sulfuric acid and
Quartz sand (silica) is chemically reacted (i.e.：By the mixture of hydrofluoric acid, sulfuric acid and quartz sand in reaction temperature 110
DEG C~130 DEG C in the environment of reacted) produce, but produce ocratation scheme by using said program there is as follows
Defect：
(one), hydrofluoric acid it is expensive, have the shortcomings that production cost is excessively high；
(secondly), prepared using the above method, need temperature being heated to 110 DEG C~130 DEG C just to have ocratation output,
Therefore haves the shortcomings that high energy consumption and preparation efficiency is low；
(thirdly), due to needing to be collected ocratation after the reaction, and the gas of output after the completion of reaction at present
Body type is more and reaction is compared with slow (including mixing effect is poor and contact surface when reacting is small), therefore there is also low production efficiencies
Defect.
Invention content
It is a kind of using prodan as raw material life in view of the deficiencies of the prior art, the present invention intends to provide
Produce the method and its production equipment of ocratation, it is intended to which solve to occur in above-mentioned background technology is unfavorable for popularization, high energy consumption system
The low defect of standby efficiency.
The technical proposal of the invention is realized in this way：A kind of side producing ocratation using prodan as raw material
Method, which is characterized in that include the following steps：
(1) it is added after mixing sulfuric acid with quartz sand into hollander tub and is stirred so that the two forms slurry；
(2) it in the whipping process to slurry, continues through nitrogen and prodan is added to reaction kettle；
(3) after prodan is added, side that the part size being uniformly mixed in hollander tub is passed through into nitrogen protection
Formula is added into reaction kettle, and the temperature in reaction kettle is heated to 60 DEG C~100 DEG C so that prodan is carried out with sulfuric acid
Reaction and output silicon tetrafluoride gas and hydrogen fluoride gas；
(4) hydrogen fluoride gas of output can dissolve and sulfuric acid and output hydrofluoric acid solution, the hydrogen fluorine of output in step (3)
Acid solution, which is further reacted with the quartz sand in reaction kettle, generates silicon tetrafluoride gas；
(5) silicon tetrafluoride gas of the output in step (3) and step (4) and hydrogen fluoride gas are passed through in scrubbing tower and are washed
It washs, dry and collect.
Preferably：The quartz sand is the silica that purity is 97%~99%, the sulfuric acid be concentration be 80%~
85% dilute sulfuric acid.
Preferably：The hydrogen fluoride gas isolated in step (5) is passed through and is reacted simultaneously with quartz sand into hollander tub
And output silicon tetrafluoride gas.
By using above-mentioned technical proposal：The first step, prodan is reacted in a kettle with sulfuric acid and output
Silicon tetrafluoride gas, hydrogen fluoride gas and sodium sulfate crystal, the silicon tetrafluoride gas of output and partially fluorinated hydrogen are logical
Enter to drying tower and be dried, will be dry after ocratation be collected, and the hydrogen fluoride gas isolated is passed through
Into hollander tub；Second step, the hydrogen fluoride and silicon dioxde reaction being passed through in hollander tub, hydrogen fluoride are generated with silicon dioxde reaction
Ocratation and water, and the ocratation generated in hollander tub is fed through in drying tower dry decomposition, by four after drying
Silicon fluoride is collected；It should be noted that：The partially fluorinated hydrogen of output can be with the titanium dioxide in reaction kettle in the first step
Silicon is reacted and generates silicon tetrafluoride gas；Preparing ocratation not only by three aspect productions has production efficiency high
The advantages of, and the hydrogen fluoride that prodan is generated with sulfuric acid reaction can be used for further utilizing again, additionally it is possible to and resource is mutual
Complementation is helped to carry out integration utilization, therefore there is also the high advantages of resource utilization；Secondly, the side by adding nitrogen protective paste to transport
Effectively air can be discharged for formula, in order to only exist three kinds of nitrogen, hydrogen fluoride and ocratation during reaction
Gas, so as to improve the decomposition efficiency to mixed gas, to further improve the preparation efficiency of ocratation；In addition
, prodan can react at normal temperatures with sulfuric acid, and reaction is best at temperature 60 C~100 DEG C, therefore there is also energy
It is enough low and the advantages of further provide for production efficiency；And the cost of prodan is relatively low, and in prodan and other substance (sulphur
Acid) reaction process in again can produce required hydrogen fluoride with output, to reduce the cost of production.
In addition, the present invention also provides a kind of production equipment producing ocratation using prodan as raw material, it is special
Sign is：Including interconnected hollander tub, reaction kettle and drying tower；It is equipped with for two between hollander tub and reaction kettle
The nitrogen feedway of person's supplying nitrogen.
Preferably：The hollander tub includes the groove body that shape is " truncated cone-shaped " and hollow setting, the both sides outer wall of the groove body
Respectively symmetrically it is communicated with conveying pipeline, the connection end of each conveying pipeline and groove body is along the inner wall circumferential direction spiral of groove body to the bottom of groove body
Feeding groove is extended to form, the free end of each feeding groove extends respectively between groove body bottom wall and the bottom wall of another feeding groove；Institute
The center for stating groove body bottom outer wall is formed with a guide post to groove body inner recess, and the outer wall of the guide post, which is connected with, to be passed through
The side wall of the swivel becket of motor-driven rotation, the groove body is equipped with the first discharge port, and the outer wall interval of the swivel becket, which is fixed, to be connected
It is connected to the mixing component for being stirred to the material inside groove body, the bottom interior wall spaced radial of the groove body is supplied equipped with multi-turn
Locating slot, the slot bottom of each locating slot are equipped at intervals with multiple recess portions to mixing component in axial sliding；The drying tower passes through air inlet pipe
It is connected to the top of groove body；The side wall of the groove body is equipped with heater.
Preferably：The mixing component includes the agitator disk being fixedly connected with swivel becket, is radially provided on the agitator disk
Multi-turn runs through the inner cavity of agitator disk and is equipped with stirring ring compatible with inner cavity, the top of the inner cavity in each interior intracavitary from top to bottom
Portion's both sides of edges is arched upward by the stirring that multiple circumferential gaps are arranged and is fixedly connected, and each top end surface for stirring ring is circumferentially-spaced to be set
There are multiple stirring tips；The bottom of the agitator disk is radially fixed to be connected with multiple locating pieces being active in inside each locating slot,
The thickness of the locating piece is equal with the height of recess portion to locating slot groove top.
Preferably：The reaction kettle includes autoclave body and the storage device that is fixed on inside the autoclave body, and the autoclave body is close
The side wall of bottom is equipped with the first charging aperture being connected to the first discharge port by material transfer pipe, and side wall of the autoclave body close to top is set
It is useful for the second charging aperture of the filling into storage device；The storage device includes the storage tank being fixedly connected with inner wall of kettle
The bottom wall of body, the storing tank body is equipped with circular open, and the circular open has extended to form sliding to the bottom direction of autoclave body and led to
Road slidably connects cylindricality block compatible with the sliding channel in the sliding channel, side of the cylindricality block close to top
Wall is circumferentially-spaced to be equipped with the second discharge port, and each second discharge port has extended to form a plurality of discharging channel to the bottom of cylindricality block,
The one end of each discharging channel far from the second discharge port is communicated with drainage conduit, each drainage conduit mutually spiral winding and to autoclave body
Bottom direction extends and is arranged to the inner circumferential wall direction jag of autoclave body, is fixedly connected at the top of the cylindricality block and passes through hydraulic pressure
The lifting shaft of cylinder driving；The side wall of the autoclave body is equipped with exhaust outlet, which is connected to by exhaust pipe with drying tower；It is described
The bottom of autoclave body is equipped with heater.
Preferably：The bottom interior wall of the storing tank body is gradually recessed setting, and storing tank body from edge to circular open
Bottom interior wall be fixedly connected with several cutting plates from the edge of circular open to circumferentially-spaced between the edge of bottom interior wall,
The bottom interior wall of storing tank body is divided by several cutting plates multiple deflector chutes, each deflector chute respectively with each second discharge port one
One corresponds to, and side of each cutting plate far from storing tank body bottom interior wall is fixedly connected with the guide that cross section is " half elliptic "
Plate.
Preferably：The discharge end of the drainage conduit can bend and be obliquely installed.
By using above-mentioned technical proposal：(one), sulfuric acid and quartz sand are (i.e.：Silica) groove body two can be passed through respectively
The conveying pipeline of side is added to the inside of groove body, and due to being equipped with the feeding groove being connected to conveying pipeline in groove body, each feeding groove can incite somebody to action
Material is transported to the bottom of groove body, the free end of each feeding groove extend respectively to groove body bottom wall and another feeding groove bottom wall it
Between, which can improve the fusion uniformity of two parts material, to improve the efficiency of stirring, and then improve ocratation
Production efficiency；Mixing component is moved after two parts material mixes by motor-driven rotation annulus to stir material
It mixes, due to the stirring tip being arranged on the inner cavity being radially arranged on agitator disk, the stirring ring being arranged on inner cavity and stirring ring, and
And the recess portion due to stirring the locating piece of pan bottom setting, the locating slot of groove body bottom setting and the setting of locating slot slot bottom,
So that locating piece moves in a circle in locating slot during agitator disk rotates, stirs when locating piece passes through recess portion and stir at this time
The bottom for mixing disk is bonded with the bottom of slot bottom, and when locating piece is detached from recess portion, the bottom of agitator disk is detached with the bottom of slot bottom, from
And so that agitator disk does elevating movement repeatedly during rotation, and then improve the stirring efficiency to material, i.e.,：It is stirring
During mixing disk elevating movement, what stirring tip can be repeatedly punctures material, stirs and arch upward meeting after material is punctured
Material is timely stirred, to easily make two kinds of materials (i.e.：Sulfuric acid and quartz sand) rapid fusion, and then by coming
The uniformly mixed efficiency to material is improved, to improve the efficiency of production；It should be noted that：It is fixed that guide post can realize swivel becket
Position effect, can be prevented during agitator disk elevating movement swivel becket be detached from guide post, to come ensure stirring it is normal into
Row；(secondly), into storage tank body feed before, cylindricality block can be risen by hydraulic cylinder and lifting shaft so that cylindricality
The bottom margin of block is overlapped with circular open, then prodan is added into storage tank body by second charging aperture, works as fluosilicic acid
Sodium addition finishes after close second charging aperture, then by material transfer pipe by the slurry of groove body interior section (i.e.：Sulfuric acid and quartz
The mixture of sand) it is added to autoclave body, after slurry is added, cylindricality block will be put down and make column by driving hydraulic cylinder
The coincident of the bottom margin and circular open of the second discharge port on shape block so that the prodan of storing tank interior is logical
It crosses discharging channel and drainage conduit enters the bottom of autoclave body and reacted with slurry；Due to each drainage conduit mutually spiral winding and
Extend to the bottom direction of autoclave body and to the inner circumferential wall direction jag setting of autoclave body, the material of storing tank interior can be distinguished
To the different zones conveying at the top of slurry, to improve the reaction efficiency of prodan and sulfuric acid, and the setting of spiral winding
The structural strength of drainage conduit can also be improved, the discharge end of drainage conduit, which can be bent, to be obliquely installed, which can make from row
The prodan being discharged in expects pipe is added into slurry at an angle, to improve the contact area of prodan and sulfuric acid,
And then to improve the efficiency of production ocratation；The bottom interior wall of storing tank body be gradually recessed from edge to circular open setting,
The stock guide being fixedly connected on several cutting plates and cutting plate that the bottom interior wall of storing tank body is fixedly connected, which can
In storing tank body discharge, prodan to be avoided to remain in storing tank interior, to improve the utilization rate of resource；And
The rate that prodan enters to discharging channel can also be improved, and then the efficiency of production can also be improved.
The present invention is further arranged to：The top of the groove body is communicated with nitrogen feedway by air supply pipe.
Preferably：The nitrogen feedway include nitrogen storage tank and for by the liquid nitrogen vaporization inside nitrogen storage tank at
The heat exchanger of nitrogen.
By using above-mentioned technical proposal：Nitrogen feedway can be passed through nitrogen into reaction kettle and hollander tub, be passed through
The purpose of nitrogen is：Remaining air inside reaction kettle and hollander tub is discharged, nitrogen, fluorination are only existed during reaction
Three kinds of gases of hydrogen and ocratation, so as to improve the efficiency of rectifying, to further improve the preparation of ocratation
Efficiency；It should be noted that：Nitrogen in reaction kettle and hollander tub is Ke Xunhuanliyong, and in air pressure inside shakiness or inspection
The nitrogen lacked can be supplied by the nitrogen feedway at the top of groove body when measuring impurity air, the nitrogen described in the part follows
Ring utilizes, i.e.,：Hydrogen fluoride, ocratation and the nitrogen that reaction kettle generates after completion of the reaction, which can be passed through together in drying tower, to carry out
Rectifying, since the gas of the boiling point of nitrogen, hydrogen fluoride and ocratation is different, after ocratation being isolated, by nitrogen
Gas and hydrogen fluoride together be passed through in hollander tub so that hydrogen fluoride is further reacted with the silica in hollander tub, to
Output ocratation, and then to improve the efficiency for preparing ocratation.
In summary：The present invention can prepare the ocratation that production refers to by three aspects：(one), prodan and sulphur
Acid carries out reaction and output silicon tetrafluoride gas and hydrogen fluoride gas in a kettle；(secondly), in one output fluorination
Hydrogen is passed through to further being reacted output ocratation again with the silica in slurry in hollander tub；(its
Three), the hydrogen fluoride gas of output can carry out reacting further generation ocratation gas with the slurry in reaction kettle in reaction kettle
Body；By output silicon tetrafluoride gas in terms of above three, to improve the production efficiency of ocratation.
Description of the drawings
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention without having to pay creative labor, may be used also for those of ordinary skill in the art
With obtain other attached drawings according to these attached drawings.
Fig. 1 is the structure diagram of the specific embodiment of the invention 2；
Fig. 2 is the structural schematic diagram of hollander tub in Fig. 1；
Fig. 3 is the A-A sectional views in Fig. 2；
Fig. 4 is the structural schematic diagram of reaction kettle in Fig. 1；
Fig. 5 is the B-B sectional views in Fig. 4.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other without creative efforts
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1
The invention discloses a kind of methods producing ocratation as raw material using prodan, which is characterized in that packet
Include following steps：
(1) it is added after mixing sulfuric acid with quartz sand into hollander tub and is stirred so that the two forms slurry；
(2) it in the whipping process to slurry, continues through nitrogen and prodan is added to reaction kettle；
(3) after prodan is added, side that the part size being uniformly mixed in hollander tub is passed through into nitrogen protection
Formula is added into reaction kettle, and the temperature in reaction kettle is heated to 60 DEG C~100 DEG C so that prodan is carried out with sulfuric acid
Reaction and output silicon tetrafluoride gas and hydrogen fluoride gas；
(4) hydrogen fluoride gas of output can dissolve and sulfuric acid and output hydrofluoric acid solution, the hydrogen fluorine of output in step (3)
Acid solution, which is further reacted with the quartz sand in reaction kettle, generates silicon tetrafluoride gas；
(5) silicon tetrafluoride gas of the output in step (3) and step (4) and hydrogen fluoride gas are passed through in scrubbing tower and are washed
It washs, dry and collect.
In the specific embodiment of the invention, the quartz sand is the silica that purity is 97%~99%, the sulfuric acid
It is 80%~85% dilute sulfuric acid for concentration.
In the specific embodiment of the invention, the hydrogen fluoride gas isolated in step (5) can be passed through into hollander tub
It is reacted with quartz sand and output silicon tetrafluoride gas.
By using above-mentioned technical proposal：The first step, prodan is reacted in a kettle with sulfuric acid and output
Silicon tetrafluoride gas, hydrogen fluoride gas and sodium sulfate crystal, the silicon tetrafluoride gas of output and partially fluorinated hydrogen are logical
Enter to drying tower and be dried, will be dry after ocratation be collected, and the hydrogen fluoride gas isolated is passed through
Into hollander tub；Second step, the hydrogen fluoride and silicon dioxde reaction being passed through in hollander tub, hydrogen fluoride are generated with silicon dioxde reaction
Ocratation and water, and the ocratation generated in hollander tub is fed through in drying tower dry decomposition, by four after drying
Silicon fluoride is collected；It should be noted that：The partially fluorinated hydrogen of output can be with the titanium dioxide in reaction kettle in the first step
Silicon is reacted and generates silicon tetrafluoride gas；Preparing ocratation not only by three aspect productions has production efficiency high
The advantages of, and the hydrogen fluoride that prodan is generated with sulfuric acid reaction can be used for further utilizing again, additionally it is possible to and resource is mutual
Complementation is helped to carry out integration utilization, therefore there is also the high advantages of resource utilization；Secondly, the side by adding nitrogen protective paste to transport
Effectively air can be discharged for formula, in order to only exist three kinds of nitrogen, hydrogen fluoride and ocratation during reaction
Gas, so as to improve the decomposition efficiency to mixed gas, to further improve the preparation efficiency of ocratation；In addition
, prodan can react at normal temperatures with sulfuric acid, and reaction is best at temperature 60 C~100 DEG C, therefore there is also energy
It is enough low and the advantages of further provide for production efficiency；And the cost of prodan is relatively low, and in prodan and other substance (sulphur
Acid) reaction process in again can produce required hydrogen fluoride with output, to reduce the cost of production.
Embodiment 2
As shown in fig. 1~fig. 5, the invention discloses a kind of productions producing ocratation using prodan as raw material
Equipment, in the specific embodiment of the invention, including interconnected hollander tub 1, reaction kettle 2 and drying tower 3；In hollander tub 1
It is equipped with for the nitrogen feedway 4 to the two supplying nitrogen between reaction kettle 2.
In the specific embodiment of the invention, the hollander tub 1 includes the groove body 11 that shape is " truncated cone-shaped " and hollow setting,
The both sides outer wall of the groove body 11 is respectively symmetrically communicated with conveying pipeline 12, and the connection end of each conveying pipeline 12 and groove body 11 is along groove body 11
Inner wall circumferential direction spiral extended to form feeding groove 13 to the bottom of groove body 11, the free end of each feeding groove 13 extends respectively to slot
Between 11 bottom wall of body and the bottom wall of another feeding groove 13；The center of 11 bottom outer wall of the groove body is formed to 11 inner recess of groove body
There is a guide post 111, the outer wall of the guide post 111 is connected with the swivel becket 113 by the driving rotation of motor 112, described
The side wall of groove body 11 is equipped with the first discharge port 14, and the outer wall interval of the swivel becket 113, which is fixedly connected, to be useful for in groove body 11
The bottom interior wall spaced radial of the mixing component 15 that the material in portion is stirred, the groove body 11 is equipped with multi-turn for 15 axis of mixing component
To the locating slot 16 of sliding, the slot bottom of each locating slot 16 is equipped at intervals with multiple recess portions 161；The drying tower 3 passes through air inlet pipe 17
It is connected to the top of groove body 11；The side wall of the groove body 11 is equipped with heater 18.
In the specific embodiment of the invention, the mixing component 15 includes the agitator disk being fixedly connected with swivel becket 113
151, it is radially provided with multi-turn on the agitator disk 151 and runs through the inner cavity 151a of agitator disk 151 from top to bottom and in each inner cavity 151a
Interior to be equipped with stirring ring 151b compatible with inner cavity 151a, the top edge both sides of the inner cavity 151a pass through multiple circumferential gaps
The stirring of the setting 151c that arches upward is fixedly connected, and each top end surface for stirring ring 151b is circumferentially-spaced to be equipped with multiple stirring tips
151d；The bottom of the agitator disk 151 is radially fixed to be connected with multiple locating piece 151e being active in inside each locating slot 16, institute
The thickness for stating locating piece 151e is equal with the height of recess portion to 16 groove top of locating slot.
In the specific embodiment of the invention, the reaction kettle 2 includes autoclave body 21 and the storage being fixed on inside the autoclave body 21
Expect device 22, the autoclave body 21 close to bottom side wall be equipped with by material transfer pipe 211 be connected to the first discharge port 14 first into
Material mouth 212, side wall of the autoclave body 21 close to top are equipped with the second charging aperture 213 for the filling into storage device 22；Institute
It includes the storing tank body 221 being fixedly connected with 21 inner wall of autoclave body to state storage device 22, and the bottom wall of the storing tank body 221 is equipped with circle
Be open 221a, and the circular open 221a has extended to form sliding channel 221b to the bottom direction of autoclave body 21, and the sliding is logical
Cylindricality block 221c compatible with the sliding channel 221b is slidably connected in road 221b, cylindricality block 221c is close to top
Side wall is circumferentially-spaced to be equipped with the second discharge port 221d, and each second discharge port 221d has been extended to form to the bottom of cylindricality block 221c
The one end of a plurality of discharging channel 221e, each discharging channel 221e far from the second discharge port 221d is communicated with drainage conduit 221f, respectively
Drainage conduit 221f mutually spiral winding and the inner circumferential wall direction jag settings to the extension of the bottom direction of autoclave body and to autoclave body,
It is fixedly connected with the lifting shaft 25 driven by hydraulic cylinder 24 at the top of the cylindricality block 221c；The side wall of the autoclave body is equipped with
Exhaust outlet 26, the exhaust outlet 26 are connected to by exhaust pipe 261 with drying tower 3；The bottom of the autoclave body 21 is equipped with heater 27.
In the specific embodiment of the invention, the bottom interior wall of the storing tank body 221 from edge to circular open 221a by
Gradually recess setting, and the bottom interior wall of storing tank body 221 is from the edge of circular open 221a to week between the edge of bottom interior wall
It is fixedly connected with several cutting plates 221g to interval, the bottom interior wall of storing tank body 221 is divided by several cutting plates 221h
There are multiple deflector chute 221k, each deflector chute 221k to be corresponded respectively with each second discharge port 221d, each cutting plate 221d is separate
The side of 221 bottom interior wall of storing tank body is fixedly connected with the stock guide 221m that cross section is " half elliptic ".
In the specific embodiment of the invention, the discharge end of the drainage conduit 221f, which can be bent, to be obliquely installed.
By using above-mentioned technical proposal：(one), sulfuric acid and quartz sand are (i.e.：Silica) groove body two can be passed through respectively
The conveying pipeline of side is added to the inside of groove body, and due to being equipped with the feeding groove being connected to conveying pipeline in groove body, each feeding groove can incite somebody to action
Material is transported to the bottom of groove body, the free end of each feeding groove extend respectively to groove body bottom wall and another feeding groove bottom wall it
Between, which can improve the fusion uniformity of two parts material, to improve the efficiency of stirring, and then improve ocratation
Production efficiency；Mixing component is moved after two parts material mixes by motor-driven rotation annulus to stir material
It mixes, due to the stirring tip being arranged on the inner cavity being radially arranged on agitator disk, the stirring ring being arranged on inner cavity and stirring ring, and
And the recess portion due to stirring the locating piece of pan bottom setting, the locating slot of groove body bottom setting and the setting of locating slot slot bottom,
So that locating piece moves in a circle in locating slot during agitator disk rotates, stirs when locating piece passes through recess portion and stir at this time
The bottom for mixing disk is bonded with the bottom of slot bottom, and when locating piece is detached from recess portion, the bottom of agitator disk is detached with the bottom of slot bottom, from
And so that agitator disk does elevating movement repeatedly during rotation, and then improve the stirring efficiency to material, i.e.,：It is stirring
During mixing disk elevating movement, what stirring tip can be repeatedly punctures material, stirs and arch upward meeting after material is punctured
Material is timely stirred, to easily make two kinds of materials (i.e.：Sulfuric acid and quartz sand) rapid fusion, and then by coming
The uniformly mixed efficiency to material is improved, to improve the efficiency of production；It should be noted that：It is fixed that guide post can realize swivel becket
Position effect, can be prevented during agitator disk elevating movement swivel becket be detached from guide post, to come ensure stirring it is normal into
Row；(secondly), into storage tank body feed before, cylindricality block can be risen by hydraulic cylinder and lifting shaft so that cylindricality
The bottom margin of block is overlapped with circular open, then prodan is added into storage tank body by second charging aperture, works as fluosilicic acid
Sodium addition finishes after close second charging aperture, then by material transfer pipe by the slurry of groove body interior section (i.e.：Sulfuric acid and quartz
The mixture of sand) it is added to autoclave body, after slurry is added, cylindricality block will be put down and make column by driving hydraulic cylinder
The coincident of the bottom margin and circular open of the second discharge port on shape block so that the prodan of storing tank interior is logical
It crosses discharging channel and drainage conduit enters the bottom of autoclave body and reacted with slurry；Due to each drainage conduit mutually spiral winding and
Extend to the bottom direction of autoclave body and to the inner circumferential wall direction jag setting of autoclave body, the material of storing tank interior can be distinguished
To the different zones conveying at the top of slurry, to improve the reaction efficiency of prodan and sulfuric acid, and the setting of spiral winding
The structural strength of drainage conduit can be improved, the discharge end of drainage conduit, which can be bent, to be obliquely installed, which can make from discharge
The prodan being discharged in pipe is added into slurry at an angle, to improve the contact area of prodan and sulfuric acid, into
And to improve the efficiency of production ocratation；The bottom interior wall of storing tank body be gradually recessed from edge to circular open setting, storage
The stock guide being fixedly connected on several cutting plates and cutting plate that the bottom interior wall of batch can body is fixedly connected, the setting can be with
In storing tank body discharge, prodan is avoided to remain in storing tank interior, to improve the utilization rate of resource；And also
The rate that prodan enters to discharging channel can be improved, and then the efficiency of production can also be improved.
In the specific embodiment of the invention, the top of the groove body 11 is communicated with nitrogen feedway 4 by air supply pipe 41.
In the specific embodiment of the invention, the nitrogen feedway 4 can be nitrogen storage tank 42 and be used for nitrogen
Liquid nitrogen vaporization inside storage tank 42 at nitrogen heat exchanger 43.
By using above-mentioned technical proposal：Nitrogen feedway can be passed through nitrogen into reaction kettle and hollander tub, be passed through
The purpose of nitrogen is：Remaining air inside reaction kettle and hollander tub is discharged, nitrogen, fluorination are only existed during reaction
Three kinds of gases of hydrogen and ocratation, so as to improve the efficiency of rectifying, to further improve the preparation of ocratation
Efficiency；It should be noted that：Nitrogen in reaction kettle and hollander tub is Ke Xunhuanliyong, and in air pressure inside shakiness or inspection
The nitrogen lacked can be supplied by the nitrogen feedway at the top of groove body when measuring impurity air, the nitrogen described in the part follows
Ring utilizes, i.e.,：Hydrogen fluoride, ocratation and the nitrogen that reaction kettle generates after completion of the reaction, which can be passed through together in drying tower, to carry out
Rectifying, since the gas of the boiling point of nitrogen, hydrogen fluoride and ocratation is different, after ocratation being isolated, by nitrogen
Gas and hydrogen fluoride together be passed through in hollander tub so that hydrogen fluoride is further reacted with the silica in hollander tub, to
Output ocratation, and then to improve the efficiency for preparing ocratation.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.
Claims (10)
1. a kind of method producing ocratation as raw material using prodan, which is characterized in that include the following steps：
(1) it is added after mixing sulfuric acid with quartz sand into hollander tub and is stirred so that the two forms slurry；
(2) it in the whipping process to slurry, continues through nitrogen and prodan is added to reaction kettle；
(3) after prodan is added, the part size being uniformly mixed in hollander tub is added by way of nitrogen protection
Enter into reaction kettle, and the temperature in reaction kettle is heated to 60 DEG C~100 DEG C so that prodan is reacted with sulfuric acid
And output silicon tetrafluoride gas and hydrogen fluoride gas；
(4) in step (3) hydrogen fluoride gas of output can dissolve with sulfuric acid and output hydrofluoric acid solution, the hydrofluoric acid of output is molten
Liquid, which is further reacted with the quartz sand in reaction kettle, generates silicon tetrafluoride gas；
(5) by the silicon tetrafluoride gas of the output in step (3) and step (4) and hydrogen fluoride gas be passed through in scrubbing tower washing,
It dries and collects.
2. the method according to claim 1 for producing ocratation as raw material using prodan, it is characterised in that：Institute
It is the silica that purity is 97%~99% to state quartz sand, and the sulfuric acid is the dilute sulfuric acid that concentration is 80%~85%.
3. the method according to claim 1 or 2 for producing ocratation as raw material using prodan, feature exist
In：The hydrogen fluoride gas isolated in step (5) is passed through into hollander tub and is reacted with quartz sand and output tetrafluoride
Silicon gas.
4. a kind of production equipment producing ocratation using prodan as raw material as described in the claims, special
Sign is：Including interconnected hollander tub, reaction kettle and drying tower；It is equipped with for two between hollander tub and reaction kettle
The nitrogen feedway of person's supplying nitrogen.
5. the production equipment according to claim 4 for being produced ocratation using prodan as raw material, feature are existed
In：The hollander tub includes the groove body that shape is " truncated cone-shaped " and hollow setting, and the both sides outer wall of the groove body is respectively symmetrically connected to
There is a conveying pipeline, the connection end of each conveying pipeline and groove body has extended to form along the inner wall circumferential direction spiral of groove body to the bottom of groove body defeated
The free end of hopper, each feeding groove extends respectively between groove body bottom wall and the bottom wall of another feeding groove；Outside the groove body bottom
The center of wall is formed with a guide post to groove body inner recess, and the outer wall of the guide post, which is connected with, passes through motor-driven rotation
Swivel becket, the side wall of the groove body is equipped with the first discharge port, and the outer wall interval of the swivel becket, which is fixedly connected, to be useful for slot
The bottom interior wall spaced radial of the mixing component that the material in internal portion is stirred, the groove body is equipped with multi-turn for mixing component axial direction
The slot bottom of the locating slot of sliding, each locating slot is equipped at intervals with multiple recess portions；The top that the drying tower passes through air inlet pipe and groove body
Connection；The side wall of the groove body is equipped with heater.
6. the production equipment according to claim 5 for being produced ocratation using prodan as raw material, feature are existed
In：The top of the groove body is communicated with nitrogen feedway by air supply pipe.
7. the production equipment for producing ocratation using prodan as raw material according to claim 4 or 6, feature
It is：The nitrogen feedway includes nitrogen storage tank and for the heat exchange by the liquid nitrogen vaporization inside nitrogen storage tank at nitrogen
Device.
8. the production equipment according to claim 5 or 6 for producing ocratation using prodan as raw material, feature
It is：The mixing component includes the agitator disk being fixedly connected with swivel becket, multi-turn is radially provided on the agitator disk from upper and
Run through the inner cavity of agitator disk down and is equipped with stirring ring compatible with inner cavity, the top edge both sides of the inner cavity in each interior intracavitary
The stirring being arranged by multiple circumferential gaps, which is arched upward, to be fixedly connected, and each top end surface for stirring ring is circumferentially-spaced to be equipped with multiple stirrings
Tip；The bottom of the agitator disk is radially fixed to be connected with multiple locating pieces being active in inside each locating slot, the locating piece
Thickness it is equal with the height of recess portion to locating slot groove top.
9. the production equipment that ocratation is produced using prodan as raw material according to claim 4 or 5 or described in 6,
It is characterized in that：The reaction kettle includes autoclave body and the storage device that is fixed on inside the autoclave body, and the autoclave body is close to bottom
Side wall is equipped with the first charging aperture being connected to the first discharge port by material transfer pipe, and side wall of the autoclave body close to top, which is equipped with, to be used for
The second charging aperture of filling into storage device；The storage device includes the storing tank body being fixedly connected with inner wall of kettle, should
The bottom wall of storing tank body is equipped with circular open, and the circular open has extended to form sliding channel to the bottom direction of autoclave body, institute
It states and slidably connects cylindricality block compatible with the sliding channel in sliding channel, side wall of the cylindricality block close to top is circumferential
It is equipped at intervals with the second discharge port, each second discharge port has extended to form a plurality of discharging channel, each discharge to the bottom of cylindricality block
The one end of channel far from the second discharge port is communicated with drainage conduit, each drainage conduit mutually spiral winding and to the bottom side of autoclave body
To extending and being arranged to the inner circumferential wall direction jag of autoclave body, it is fixedly connected at the top of the cylindricality block and is driven by hydraulic cylinder
Dynamic lifting shaft；The side wall of the autoclave body is equipped with exhaust outlet, which is connected to by exhaust pipe with drying tower；The autoclave body
Bottom is equipped with heater.
10. the production equipment according to claim 9 for being produced ocratation using prodan as raw material, feature are existed
In：The bottom interior wall of the storing tank body is gradually recessed setting from edge to circular open, and the bottom interior wall of storing tank body from
The edge of circular open is fixedly connected with several cutting plates to circumferentially-spaced between the edge of bottom interior wall, several cutting plates
The bottom interior wall of storing tank body, which is divided into, multiple deflector chutes, and each deflector chute is corresponded with each second discharge port respectively, each point
Side of the flitch far from storing tank body bottom interior wall is fixedly connected with the stock guide that cross section is " half elliptic ".
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