CN115259198A - Dry treatment process and equipment for high-calcium-carbonate fluorite powder - Google Patents
Dry treatment process and equipment for high-calcium-carbonate fluorite powder Download PDFInfo
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- CN115259198A CN115259198A CN202210884580.XA CN202210884580A CN115259198A CN 115259198 A CN115259198 A CN 115259198A CN 202210884580 A CN202210884580 A CN 202210884580A CN 115259198 A CN115259198 A CN 115259198A
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- calcium carbonate
- fluorite powder
- fluosilicic acid
- screw conveyor
- hobbing
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 214
- 229910000019 calcium carbonate Inorganic materials 0.000 title claims abstract description 112
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 title claims abstract description 93
- 239000010436 fluorite Substances 0.000 title claims abstract description 89
- 239000000843 powder Substances 0.000 title claims abstract description 83
- 238000000034 method Methods 0.000 title claims description 19
- 230000008569 process Effects 0.000 title claims description 17
- 229960003563 calcium carbonate Drugs 0.000 title description 88
- 239000002253 acid Substances 0.000 claims abstract description 93
- 229910001868 water Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims description 30
- 238000003860 storage Methods 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 17
- 239000000126 substance Substances 0.000 claims description 17
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 7
- 239000001569 carbon dioxide Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- 229910000975 Carbon steel Inorganic materials 0.000 claims description 3
- 239000010962 carbon steel Substances 0.000 claims description 3
- 238000004891 communication Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 230000008676 import Effects 0.000 claims 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 abstract description 51
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract description 26
- 238000004519 manufacturing process Methods 0.000 abstract description 22
- 229910000040 hydrogen fluoride Inorganic materials 0.000 abstract description 11
- 238000005188 flotation Methods 0.000 abstract description 7
- 239000006227 byproduct Substances 0.000 abstract description 6
- 239000000428 dust Substances 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 6
- 229910001634 calcium fluoride Inorganic materials 0.000 abstract description 5
- 239000000047 product Substances 0.000 abstract description 3
- 235000010216 calcium carbonate Nutrition 0.000 description 79
- 230000001105 regulatory effect Effects 0.000 description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 229910003638 H2SiF6 Inorganic materials 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 229910052925 anhydrite Inorganic materials 0.000 description 2
- 229960005069 calcium Drugs 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- HIFJUMGIHIZEPX-UHFFFAOYSA-N sulfuric acid;sulfur trioxide Chemical compound O=S(=O)=O.OS(O)(=O)=O HIFJUMGIHIZEPX-UHFFFAOYSA-N 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- ZEFWRWWINDLIIV-UHFFFAOYSA-N tetrafluorosilane;dihydrofluoride Chemical compound F.F.F[Si](F)(F)F ZEFWRWWINDLIIV-UHFFFAOYSA-N 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/22—Fluorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a dry processing technology and equipment for high calcium carbonate fluorite powder, wherein calcium carbonate in the fluorite powder is removed by reacting a byproduct fluosilicic acid with calcium carbonate. The purity of the raw material calcium fluoride entering the furnace in the hydrogen fluoride production can be improved; dust blockage of the condenser is reduced, and smooth production of anhydrous hydrofluoric acid is guaranteed; the consumption of sulfuric acid is reduced, and the cost is reduced; the water content of the anhydrous hydrogen fluoride of the main product is greatly reduced, the production quality of the anhydrous hydrofluoric acid is improved, and a foundation is laid for producing high-purity hydrofluoric acid; solves the problem of great difficulty of fluorite mine flotation manufacturers, and has higher economic value.
Description
Technical Field
The invention relates to the technical field of hydrofluoric acid production, in particular to a dry treatment process and equipment for high-calcium-carbonate fluorite powder.
Background
At present, the content of calcium fluoride in acid-grade fluorite used for producing hydrofluoric acid is more than 97%, the content of silicon dioxide is less than 1.5%, and the content of calcium carbonate is less than 1%. However, after part of fluorite ore is floated, the content of calcium carbonate in fluorite fine powder is about 1.5-4%, which seriously affects the production of hydrogen fluoride factories and mainly has the following disadvantages:
1. the calcium carbonate entering the converter and the sulfuric acid react violently to generate carbon dioxide, water and calcium sulfate, the moisture content of the anhydrous hydrogen fluoride can be greatly improved, and a large amount of 105% sulfuric acid (fuming sulfuric acid) is consumed;
2. the moisture generated by the reaction increases the corrosion of equipment, and in order to eliminate the influence of moisture, fuming sulfuric acid is used for absorbing moisture to prepare 100 percent sulfuric acid, so that the corrosion of the equipment is reduced;
3. the calcium carbonate content is high, the reaction speed of sulfuric acid and fluorite powder is accelerated, dust caused by violent reaction is easy to block an air duct and a cooling and rectifying system, a reaction furnace emits smoke, the production is interrupted, and environmental protection accidents are caused.
The fluorite powder with high calcium carbonate content has great influence on the production of hydrofluoric acid, so that the requirement on the calcium carbonate content in the fluorite powder is less than 1 percent in the hydrofluoric acid industry.
The effective separation of calcium carbonate in the high-calcium carbonate fluorite powder is a problem which troubles the industry for many years, the conventional flotation is difficult to be effective, and the common treatment mode of most fluorite mines for the high-calcium carbonate fluorite powder is as follows: the calcium carbonate inhibitor (a compound preparation XH 202) is added in the flotation process to realize the flotation separation of fluorite and calcium carbonate, but the defects are also obvious and mainly reflected in the following aspects:
1. the cost of the compound preparation is high;
2. adding the composite preparation requires modification of the existing flotation process;
3. the composite preparation is difficult to be highly contacted and combined with the ore pulp even under the stirring condition, and the effect is poor.
Therefore, how to effectively separate calcium carbonate from high calcium carbonate fluorite powder is a technical problem to be solved, and a new way or equipment needs to be provided to solve the problem.
Disclosure of Invention
Therefore, the invention provides a dry treatment process and equipment for high calcium carbonate fluorite powder, which aims to solve the technical problems.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention provides dry processing equipment for high-calcium carbonate fluorite powder, which comprises a fluosilicic acid pipeline, a first screw conveyor, a first storage bin and a control system, wherein an electromagnetic flow meter and a pneumatic regulating valve are connected in series on the fluosilicic acid pipeline, a fluorite powder inlet, an acid inlet and an exhaust port are sequentially arranged on the first screw conveyor according to the material flow direction, at least a stirring tooth is arranged on a spiral groove between the acid inlet and the exhaust port, the fluorite powder inlet of the first screw conveyor is connected with a discharge port of the first storage bin, the acid inlet of the first screw conveyor is connected with a discharge port of the fluosilicic acid pipeline, the control system is respectively connected with the first screw conveyor and the pneumatic regulating valve in a control mode and is in communication connection with the electromagnetic flow meter, and the control system regulates the rotating speed of the first screw conveyor and the opening degree of the pneumatic regulating valve after calculation according to the calcium carbonate content, so that the molar ratio of the fluosilicic acid to the calcium carbonate is close to 1.
Furthermore, the fluosilicic acid pipeline is a fluorine-lined carbon steel pipeline; the first outer barrel of the first screw conveyor is made of SUS316, the first screw shaft, the first screw blade and the stirring teeth of the first screw conveyor are made of Ha C-276 materials, and the motor of the first screw conveyor is a variable-frequency speed regulating motor and is electrically connected with the control system.
Furthermore, a convex shell protruding upwards is arranged on the first outer cylinder of the first spiral conveyor, the space in the convex shell is communicated with the space in the first outer cylinder, and the air outlet is formed in the convex shell.
Furthermore, a manual valve and a pneumatic cut-off ball valve are connected to the fluosilicic acid pipeline in series, and the control system is in control connection with the pneumatic cut-off ball valve.
Furthermore, the dry processing equipment for the high calcium carbonate fluorite powder further comprises a first double-hobbing-gear blanking machine, two hobbing parts of the first double-hobbing-gear blanking machine are arranged in a discharge port below the first storage bin, and a motor of the first double-hobbing-gear blanking machine adopts a variable frequency speed regulating motor and is electrically connected with the control system.
Further, the dry processing equipment for high calcium carbonate fluorite powder further comprises a fluosilicic acid storage tank and a chemical pump, wherein a liquid inlet of the chemical pump is connected with the fluosilicic acid storage tank, a liquid outlet of the chemical pump is connected with a liquid inlet of the fluosilicic acid pipeline, and the chemical pump is electrically connected with the control system.
Further, the dry processing equipment of high calcium carbonate fluorite powder still includes second feed bin, the two hobbing cutter blanking machines of second, second screw conveyer and stoving converter, first screw conveyer's discharge gate with the feed inlet process of second feed bin is connected, two hobbing cutter portions of the two hobbing cutter blanking machines of second set up in the discharge gate of second feed bin below, the motor of the two hobbing cutter blanking machines of second adopt variable frequency speed governing motor and with the control system electricity is connected, the discharge gate of second feed bin with the feed inlet of second screw conveyer is connected, the discharge gate of second screw conveyer with the feed inlet of stoving converter is connected.
The second aspect of the present invention provides a dry processing technique for high calcium carbonate fluorite powder, which adopts the dry processing equipment according to the first aspect of the present invention, and comprises the following steps:
calculating the supply amount of high calcium carbonate fluorite powder and fluosilicic acid according to the content of calcium carbonate, so that the molar ratio of the fluosilicic acid to the calcium carbonate is close to 1;
adjusting the rotating speed of the first screw conveyor and the opening of a pneumatic adjusting valve according to the calculation result, and supplying high calcium carbonate fluorite powder and fluosilicic acid into the first screw conveyor;
stirring and mixing the high-calcium-carbonate fluorite powder and the fluosilicic acid in a first screw conveyor, and simultaneously carrying out chemical reaction on the calcium carbonate and the fluosilicic acid;
carbon dioxide generated during the chemical reaction is exhausted from the exhaust port.
Further, the dry treatment process of the high calcium carbonate fluorite powder also comprises the following steps:
high calcium carbonate fluorite powder and fluosilicic acid in the first screw conveyer are mixed, and the mixture after reaction is sent to a second bin;
adjusting the rotating speed of the second double-hobbing blanking machine and the second screw conveyor, and conveying the high-water-content fluorite powder subjected to calcium carbonate removal in the second bin to the drying converter at a certain speed;
and drying the high-water-content fluorite powder subjected to calcium carbonate removal in a drying converter, and removing water.
The invention has the following advantages:
the byproduct fluosilicic acid generated in the hydrogen fluoride production is reacted with calcium carbonate in high-calcium carbonate fluorite powder to remove the calcium carbonate in the fluorite powder, so that the purity of the raw material calcium fluoride entering the furnace in the hydrogen fluoride production is improved, and the raw material impurities are reduced; because calcium carbonate is removed, dust caused by violent reaction of sulfuric acid and fluorite powder can not appear in the subsequent production process, the dust blockage of a condenser is reduced, and the smooth production of anhydrous hydrofluoric acid is ensured; after the calcium carbonate is removed, the condition that water is generated by the reaction of the calcium carbonate and sulfuric acid is avoided, the consumption of the sulfuric acid is reduced, the cost is reduced, the moisture content of a main product is greatly reduced, the production quality of anhydrous hydrofluoric acid is improved, and a foundation is laid for producing high-purity hydrofluoric acid; solves the problem of the old and difficult problem of fluorite mine flotation manufacturers, and has higher economic value.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It should be apparent that the drawings in the following description are merely exemplary, and that other embodiments can be derived from the drawings provided by those of ordinary skill in the art without inventive effort.
The structures, ratios, sizes, and the like shown in the present specification are only used for matching with the contents disclosed in the specification, so that those skilled in the art will understand and read the present invention, and do not limit the conditions for implementing the present invention, so that the present invention has no technical essence, and any modifications of the structures, changes of the ratio relationships, or adjustments of the sizes, should still fall within the scope covered by the technical contents disclosed in the present invention without affecting the efficacy and the achievable purpose of the present invention.
FIG. 1 is a schematic diagram of a dry processing apparatus for high calcium carbonate fluorite powder according to an embodiment of the present invention;
fig. 2 is a schematic connection diagram of a first bunker, a first screw conveyor and a second bunker of the dry processing equipment for high calcium carbonate fluorite powder according to the embodiment of the present invention;
FIG. 3 is an enlarged view of a portion of FIG. 2;
fig. 4 is an electric control schematic diagram of the dry processing equipment for high calcium carbonate fluorite powder according to the embodiment of the present invention.
In the figure: 1-fluosilicic acid storage tank, 2-chemical pump, 3-fluosilicic acid pipeline, 4-first storage bin, 5-first double-hobbing cutter blanking machine, 6-first screw conveyor, 7-second storage bin, 8-second double-hobbing cutter blanking machine, 9-second screw conveyor, 10-drying converter, 11-control system, 12-manual valve, 13-electromagnetic flowmeter, 14-pneumatic regulating valve, 15-pneumatic cut-off ball valve, 101-rolling shaft, 102-hobbing cutter, 201-first outer barrel, 202-first screw shaft, 203-first screw blade, 204-stirring tooth, 301-fluorite powder inlet, 302-acid inlet, 303-convex shell and 304-exhaust port.
Detailed Description
The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the present specification, the terms "upper", "lower", "left", "right", "middle", and the like are used for clarity of description, and are not intended to limit the scope of the present invention, and changes or modifications in the relative relationship thereof may be made without substantial technical changes.
The embodiment provides a dry treatment process and equipment for high-calcium-carbonate fluorite powder, which are used for carrying out dry comprehensive treatment in a hydrofluoric acid factory, fully utilizing the reaction between byproduct fluosilicic acid and calcium carbonate, and greatly reducing the calcium carbonate in the fluorite powder before drying.
The following problems need to be solved:
1. designing reaction equipment for fluosilicic acid and wet fluorite powder;
2. mixing and drying the reacted fluorite powder and qualified fluorite powder;
3. the control problem of quantitative reaction between the high calcium carbonate and the fluosilicic acid;
4. the corrosion resistance of process equipment.
During the production of hydrofluoric acid, a considerable amount of by-product fluosilicic acid is generated at the same time, the content of the fluosilicic acid is about 35-40% after washing, the content of calcium carbonate is reduced by utilizing the reaction of the fluosilicic acid and calcium carbonate, and the reaction equation is as follows:
H2SiF6+3CaCO3→3CaF2+SiO2+3CO2+H2O；
the following two reactions occur during hydrofluoric acid production:
CaF2+H2SO4→CaSO4+2HF；
6HF+SiO2→H2SiF6+2H2O；
from the above chemical reaction formula, it is known that:
CaCO3+H2SO4→CaSO4+CO2+H2O；
as can be seen from the above, the whole circulation is the reaction of sulfuric acid and calcium carbonate, and the cost of calcium reduction is lower.
From the above, it is known that the dry treatment of calcium carbonate in a hydrofluoric acid plant can be performed with perfect results.
The process and equipment are described in detail below.
As shown in fig. 1 to 4, the apparatus includes a fluosilicic acid storage tank 1, a chemical pump 2, a fluosilicic acid pipeline 3, a first bunker 4, a first double-hobbing-cutter feeder 5, a first screw conveyor 6, a second bunker 7, a second double-hobbing-cutter feeder 8, a second screw conveyor 9, a drying converter 10, and a control system 11.
The fluosilicic acid storage tank 1 is used for storing fluosilicic acid generated in the production process of hydrofluoric acid, can be a container such as a tank, a tank and a barrel which do not react with the fluosilicic acid, can be connected with a hydrofluoric acid production line through a pipeline, and directly drains the fluosilicic acid into the fluosilicic acid storage tank 1.
The chemical pump 2 is arranged beside the fluosilicic acid storage tank 1, the feed inlet of the chemical pump is communicated with the fluosilicic acid storage tank 1 through a pipeline, and a valve and the like can be connected on the pipeline in series. The discharge port of the chemical pump 2 is connected with the fluosilicic acid pipeline 3, can be directly connected and can also be connected through other corrosion-resistant pipelines. The chemical pump 2 is electrically connected with the control system 11 and is controlled by the control system 11; during operation, fluosilicic acid is pumped into a fluosilicic acid pipeline 3 and then enters a first screw conveyor 6.
The first storage bin 4 is used for storing high calcium carbonate fluorite powder without decalcification, and a feed inlet of the first storage bin faces upwards, and a discharge outlet of the first storage bin faces downwards. The high calcium carbonate fluorite powder (containing water) as a raw material is in a bulk state and has poor fluidity, so that the high calcium carbonate fluorite powder needs to be fed by a double-roller-tooth feeding machine.
The structure of two hobbing cutter blanking machines is basically the same, all include the motor and with motor drive two hobbing cutter 102 portions of being connected, every hobbing cutter 102 portion all includes the roller bearing 101 of being connected with motor drive and installs a plurality of hobbing cutters 102 of thorn form on roller bearing 101, hobbing cutter 102 portion transversely sets up in the feed opening of feed bin, the hobbing cutter 102 intercrossing of two hobbing cutter 102 portions and the rotation opposite direction of two hobbing cutter 102 portions, the during operation can be with the high calcium carbonate fluorite powder of bulk from the top down the back off, thereby accomplish the unloading smoothly. The motor of the double-hobbing blanking machine adopts a variable frequency speed regulating motor, and can be regulated to the required rotating speed within a certain range under the control of the control system 11. The hob 102 of the first double-hob blanking machine 5 is located in the discharge opening of the first silo 4 and the hob 102 of the second double-hob blanking machine 8 is located in the discharge opening of the second silo 7.
One end (a feed inlet) of a fluosilicic acid pipeline 3 is connected with the chemical pump 2, the other end (a discharge outlet) of the fluosilicic acid pipeline 3 is connected with an acid inlet 302 of the first screw conveyer 6, and a manual valve 12, an electromagnetic flowmeter 13, a pneumatic regulating valve 14 and a pneumatic cut-off ball valve 15 are sequentially connected on the fluosilicic acid pipeline 3 in series according to the direction pointing out from the feed inlet to the discharge outlet; the manual valve 12 is used for manually controlling the opening and the on-off; the electromagnetic flow meter 13 is used for measuring the flow of the fluosilicic acid; the pneumatic regulating valve 14 is controlled by the control system 11 to regulate the flow rate, and the control system 11 is generally electrically connected with a positioner which controls the on-off or flow of compressed air so as to control the opening of the pneumatic regulating valve 14; the pneumatic cut-off ball valve 15 is used for controlling on-off and is also controlled by the control system 11, the general control system 11 is electrically connected with an electromagnetic valve, and the electromagnetic valve controls on-off of compressed air so as to control on-off of the pneumatic cut-off ball valve 15; the fluosilicic acid pipeline 3 is a fluorine-lined carbon steel pipeline so as not to be corroded by fluosilicic acid.
The screw conveyer comprises an outer barrel, a motor fixed at the end part of the outer barrel, a screw shaft in transmission connection with the motor and positioned in the outer barrel, and a screw blade spirally arranged on the screw shaft, wherein the motor adopts a variable frequency speed regulating motor and is electrically connected with the control system 11, and can be regulated to a required rotating speed within a certain range under the control of the control system 11. The first screw conveyor 6 has a material transferring function and is also a reaction site for fluosilicic acid and calcium carbonate, so that the first outer cylinder 201 is provided with a fluorite powder inlet 301, and an acid inlet 302 and an exhaust port 304 are sequentially arranged at the downstream of the fluorite powder inlet 301; a discharge port of the first bin 4 is connected with a fluorite powder inlet 301 on the first outer cylinder 201; the discharge hole of the fluosilicic acid pipeline 3 is connected with an acid inlet 302 on the first outer cylinder 201; the first outer barrel 201 of this section, which contains the acid inlet 302 and the vent 304, is a reaction site for fluorosilicic acid and calcium carbonate; the first outer barrel 201 at the exhaust port 304 is provided with a convex shell 303 protruding upwards, the space in the convex shell 303 is communicated with the space in the first outer barrel 201, the exhaust port 304 is arranged on the convex shell 303, and carbon dioxide generated by reaction is collected at the convex shell 303 and exhausted from the exhaust port 304; in this embodiment, two chimney-shaped exhaust ports 304 are arranged side by side on the convex shell 303; the first screw conveyor 6 further comprises a plurality of stirring teeth 204, the stirring teeth 204 are fixed on the first screw shaft 202 in the reaction site and are positioned in a spiral groove formed by the first screw blade 203, and the plurality of stirring teeth 204 are uniformly distributed in the spiral groove, so that the high-calcium-carbonate fluorite powder and the fluosilicic acid can be fully mixed, the fluosilicic acid and the fluorite powder are fully contacted and reacted, and the calcium carbonate is completely consumed; the first outer cylinder 201 is made of SUS316L, and the first screw shaft 202, the first screw blade 203 and the stirring teeth 204 are made of HAC-276 materials so as to resist corrosion of fluosilicic acid. The second screw conveyor 9 is used only for transferring the material and is not a reaction site, so that a conventional screw conveyor may be used.
The discharge gate of first screw conveyer 6 with the feed inlet process of second feed bin 7 is connected, the discharge gate of second feed bin 7 with the feed inlet of second screw conveyer 9 is connected, the discharge gate of second screw conveyer 9 with the feed inlet of stoving converter 10 is connected.
The control system 11 adopts a DCS system of a hydrofluoric acid factory, the control system 11 is respectively electrically connected with a positioner on the gas path of the chemical pump 2 and the pneumatic regulating valve 14, an electromagnetic valve on the gas path of the pneumatic cut-off ball valve 15, a motor of the first double-hobbing-cutter blanking machine 5, a motor of the first screw conveyor 6, a motor of the second double-hobbing-cutter blanking machine 8 and a motor of the second screw conveyor 9 to control the operation of the above parts, and the control system 11 is in communication connection (for example, connected through a signal line) with the electromagnetic flow meter 13 to obtain the supply amount of the fluosilicic acid. Parameter adjustments may be made in the control system 11, such as modifying the calcium carbonate content in the fluorite powder, the delivery capacity of the screw conveyor, and the flow rate of the fluorosilicic acid, such that the calcium carbonate can be completely reacted according to a molar ratio of fluorosilicic acid to calcium carbonate of 1. In order to make the operation simpler and the control more intelligent, the control system 11 can perform automatic calculation, and adjust the rotation speed of the first screw conveyor 6 (the supply amount of the fluorite powder can be adjusted) and the opening degree of the pneumatic adjusting valve 14 (the supply amount of the fluosilicic acid can be adjusted) according to the calculation result; during automatic calculation, the control system 11 calls the input calcium carbonate content, calculates the supply amount of the fluosilicic acid and the fluorite powder according to the molar ratio of the fluosilicic acid to the calcium carbonate being 1, and further calculates the opening degree of the pneumatic regulating valve 14 under the normal operation of the chemical pump 2 and the rotating speed of the first screw conveyor 6 under the normal operation of the first double-hobbing blanking machine 5. Under the action of the control system 11, the motor current of the first screw conveyor 6 and the flow measured by the electromagnetic flowmeter 13 form a proportional relation to form micro-integral PID regulation; the flow measured by the electromagnetic flowmeter 13 and the pneumatic regulating valve 14 form calculus PID regulation; the acid feeding amount changes along with the powder feeding amount, and the molar ratio of the fluosilicic acid to the calcium carbonate can be automatically adjusted to be 1.
The process adopts the device, the nodular fluorite powder is fed by a first double-hobbing machine feeding machine in a first bin, the first double-hobbing machine feeding machine adopts variable frequency speed regulation and is fed to a first spiral conveyer, a reaction area is arranged in the middle of the first conveyer, fluosilicic acid is quantitatively supplied to the upper part of the reaction area according to the calcium carbonate content, carbon dioxide gas after reaction is discharged through an exhaust pipe, the rest material enters the existing fluorite powder bin (a second bin) of a hydrofluoric acid factory, is fed into the second spiral conveyer by the second double-hobbing machine feeding machine again and is transferred into a drying furnace for drying; the supply of the fluosilicic acid is realized by implementing the PID of DCS through an adjusting valve and an electromagnetic flow meter according to the calcium carbonate content of the fluorite powder, so that the flow of the fluosilicic acid is adjusted to meet the quality requirement.
The process specifically comprises the following steps:
step S1, manually inputting the calcium carbonate content of the high calcium carbonate fluorite powder, and controlling a system to store the calcium carbonate content value for calling.
And S2, calculating the supply amount of the high calcium carbonate fluorite powder and the fluosilicic acid so that the molar ratio of the fluosilicic acid to the calcium carbonate is close to 1. In the step, manual calculation can be carried out, and then the corresponding supply quantity is input into a control system; preferably, a control system automatic calculation mode is adopted, the stored calcium carbonate content numerical value is automatically called, the supply amount of the fluosilicic acid and the fluorite powder is calculated according to the molar ratio of the fluosilicic acid to the calcium carbonate being 1.
And S3, adjusting the rotating speed of the first screw conveyer and the opening of the pneumatic adjusting valve according to the calculation result, and supplying high calcium carbonate fluorite powder and fluosilicic acid to the first screw conveyer to ensure that the molar ratio of the fluosilicic acid to the calcium carbonate fed into the first screw conveyer is 1. In this step, a form of manual adjustment may be adopted; preferably, the control system is used for automatic control and adjustment.
And S4, uniformly stirring the high carbonic acid and the fluosilicic acid in the reaction area of the first screw conveyer, reacting the mixed fluosilicic acid and calcium carbonate, discharging generated carbon dioxide from an exhaust port, and mixing generated water in the fluorite powder.
And S5, sending the high-water-content fluorite powder subjected to calcium carbonate removal to a second bin.
And S6, conveying the high-water-content fluorite powder subjected to calcium carbonate removal in the second storage bin to a drying converter at a certain speed under the action of a second double-hobbing blanking machine and a second screw conveyor.
And S7, drying and dewatering the high-water-content fluorite powder subjected to calcium carbonate removal in a drying converter.
Except that calcium carbonate is consumed by using a byproduct fluosilicic acid generated in the production of hydrogen fluoride, hydrochloric acid can be used for removing calcium.
The by-product fluosilicic acid generated in the hydrogen fluoride production is reacted with calcium carbonate in high calcium carbonate fluorite powder to remove the calcium carbonate in the fluorite powder, improve the purity of the raw material calcium fluoride entering the furnace in the hydrogen fluoride production, and reduce raw material impurities (calcium carbonate); because calcium carbonate is removed, dust caused by violent reaction of sulfuric acid and fluorite powder can not appear in the subsequent production process, the dust blockage of a condenser is reduced, and the smooth production of anhydrous hydrofluoric acid is ensured; after the calcium carbonate is removed, the condition that water is generated by the reaction of the calcium carbonate and sulfuric acid can not occur, the consumption of the sulfuric acid is reduced, the cost is reduced, meanwhile, the moisture content of a main product (anhydrous hydrogen fluoride) is greatly reduced, the production quality of the anhydrous hydrogen fluoride is improved, and a foundation is laid for producing high-purity hydrofluoric acid; solves the problem of the old and difficult problem of fluorite mine flotation manufacturers, and has higher economic value.
Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (9)
1. The utility model provides a dry processing equipment of high calcium carbonate fluorite powder, its characterized in that, includes fluosilicic acid pipeline, first screw conveyer, first feed bin and control system, electromagnetic flow meter and pneumatic control valve have concatenated on the fluosilicic acid pipeline, fluorite powder import, sour import and gas vent have been equipped with in proper order according to the material flow direction on the first screw conveyer, are equipped with the stirring tooth on the helicla flute between sour import and gas vent at least, the fluorite powder import of first screw conveyer with the discharge gate of first feed bin is connected, the sour import of first screw conveyer with the discharge gate of fluosilicic acid pipeline is connected, control system respectively with first screw conveyer, pneumatic control valve control connection and with electromagnetic flow meter communication connection, control system adjusts the rotational speed of first screw conveyer and the aperture of pneumatic control valve after the calculation according to calcium carbonate content to make the mole ratio of fluosilicic acid and calcium carbonate be close to 1.
2. The dry processing equipment for high calcium carbonate fluorite powder according to claim 1, wherein the fluosilicic acid pipeline is a fluorine-lined carbon steel pipeline; the first outer barrel of the first screw conveyor is made of SUS316L, the first screw shaft, the first screw blade and the stirring teeth of the first screw conveyor are made of Ha C-276 materials, and the motor of the first screw conveyor is a variable-frequency speed-regulating motor and is electrically connected with the control system.
3. The apparatus for dry processing of fluorite powder with high calcium carbonate according to claim 1, wherein said first outer drum of said first screw conveyor is provided with a convex shell protruding upward, a space inside said convex shell being communicated with a space inside said first outer drum, and said exhaust port being provided on said convex shell.
4. The dry processing equipment for high calcium carbonate fluorite powder as claimed in claim 1, wherein a manual valve and a pneumatic cut-off ball valve are connected in series on the fluosilicic acid pipeline, and the control system is in control connection with the pneumatic cut-off ball valve.
5. The dry processing equipment for high calcium carbonate fluorite powder according to claim 1, further comprising a first double-hobbing blanking machine, wherein two hobbing parts of the first double-hobbing blanking machine are arranged in a discharge port below the first storage bin, and a motor of the first double-hobbing blanking machine adopts a variable frequency speed control motor and is electrically connected with the control system.
6. The dry processing equipment for high calcium carbonate fluorite powder according to claim 1, further comprising a fluosilicic acid storage tank and a chemical pump, wherein a liquid inlet of the chemical pump is connected with the fluosilicic acid storage tank, a liquid outlet of the chemical pump is connected with a liquid inlet of the fluosilicic acid pipeline, and the chemical pump is electrically connected with the control system.
7. The dry processing equipment for high calcium carbonate fluorite powder according to claim 1, further comprising a second bin, a second double-hobbing-gear blanking machine, a second screw conveyor and a drying converter, wherein the discharge hole of the first screw conveyor is connected with the feed hole of the second bin in a working procedure, two hobbing parts of the second double-hobbing-gear blanking machine are arranged in the discharge hole below the second bin, the motor of the second double-hobbing-gear blanking machine adopts a variable frequency speed control motor and is electrically connected with the control system, the discharge hole of the second bin is connected with the feed hole of the second screw conveyor, and the discharge hole of the second screw conveyor is connected with the feed hole of the drying converter.
8. A dry treatment process of high calcium carbonate fluorite powder, characterized in that the dry treatment equipment according to any one of claims 1 to 7 is adopted, and the dry treatment process comprises the following steps:
calculating the supply amount of high calcium carbonate fluorite powder and fluosilicic acid according to the content of calcium carbonate, so that the molar ratio of the fluosilicic acid to the calcium carbonate is close to 1;
adjusting the rotating speed of the first screw conveyor and the opening of a pneumatic adjusting valve according to the calculation result, and supplying high calcium carbonate fluorite powder and fluosilicic acid into the first screw conveyor;
stirring and mixing the high calcium carbonate fluorite powder and the fluosilicic acid in a first screw conveyer, and simultaneously carrying out chemical reaction on the calcium carbonate and the fluosilicic acid;
carbon dioxide generated during the chemical reaction is exhausted from the exhaust port.
9. The dry processing process of fluorite powder with high calcium carbonate according to claim 8,
high calcium carbonate fluorite powder and fluosilicic acid in the first screw conveyer are mixed, and the mixture after reaction is sent to a second bin;
adjusting the rotating speed of the second double-hobbing blanking machine and the second screw conveyor, and conveying the high-water-content fluorite powder subjected to calcium carbonate removal in the second bin to the drying converter at a certain speed;
and drying the high-water-content fluorite powder subjected to calcium carbonate removal in a drying converter, and removing water.
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Application publication date: 20221101 |