CN106517246A - Method for continuously producing sodium fluoride - Google Patents
Method for continuously producing sodium fluoride Download PDFInfo
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- CN106517246A CN106517246A CN201611026307.4A CN201611026307A CN106517246A CN 106517246 A CN106517246 A CN 106517246A CN 201611026307 A CN201611026307 A CN 201611026307A CN 106517246 A CN106517246 A CN 106517246A
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- sodium fluoride
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- soda ash
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/02—Fluorides
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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
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- 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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Abstract
The invention discloses a method for continuously producing sodium fluoride, which comprises the steps of sequentially and continuously adding a sodium fluosilicate solution with the mass fraction of 20-30% and a soda ash solution with the mass fraction of 20-30% into a tubular reactor, controlling the reaction temperature to be 60-100 ℃, carrying out double decomposition reaction to generate sodium fluoride and silicon dioxide slurry, continuously entering a multi-stage flotation device for flotation, respectively obtaining slurry containing sodium fluoride and slurry containing silicon dioxide after flotation, and respectively centrifuging, washing and drying to obtain a sodium fluoride product and a silicon dioxide product; wherein the solutions obtained by centrifugation are combined and recycled as mother liquor. The invention adopts the large excess addition of the sodium carbonate in the reaction process, so that the sodium fluosilicate is fully reacted, and the conversion rate reaches 100 percent. The purity of the sodium fluoride produced by the method is more than 98.5 percent, and the purity of the silicon dioxide is more than 98.0 percent. The method has the advantages of small production scale investment, realization of automatic control, reduction of labor intensity of workers, high product quality and low raw material consumption.
Description
Technical field
The present invention relates to chemical technology field, more particularly to a kind of method of continuous production sodium fluoride.
Background technology
It is traditional with prodan and soda ash be to be given birth to using batch process as the method that raw material produces sodium fluoride and silica
Produce, production scale is little, high labor intensive, consume high, poor product quality.Concrete implementation process is：(1) mother liquor or water are put into
Put into solid soda ash in dissolving tank under agitation, after heating for dissolving, proceed to head tank, concentration 20-22% soda ash solution；(2) will
Solid prodan is put under agitation in mother liquor or water input pulping tank, is prepared as the prodan that solid content is 20-30%
Slurry, proceeds in reactor；(3) start reactor agitator, be heated to 60-80 DEG C, soda ash solution is gradually added, control
PH7.5-8 is terminal (control mol ratio 1：2) will be rinsed with mother liquor in, being put into washbasin；(4) again by the sodium fluoride employment in washbasin
Work is shoveled and is centrifuged into centrifuge, is dried and is obtained sodium fluoride product；(5) silica for rinsing out is sent from scheming is carried out
Centrifugation goes out silica, obtains silica product after drying.
Traditional production sodium fluoride technological process block-diagram is as shown in Figure 1.Chemical equation：
2Na2CO3+Na2SiF6+nH20=6NaF ↓+SiO2.nH20+2CO2↑
High containing silica in the sodium fluoride product that traditional method is produced, of poor quality, intermittently operated in addition, work are strong
Degree is big, while because washing sodium fluoride by the way of rinsing, in the wash water containing solid silica, thin sodium fluoride is more, Jing centrifugations point
It is many containing thin sodium fluoride in the silica solid for separating out, cause the loss of material, consumption to increase, the silica produced is produced
Quality is poor.
The present invention is of poor quality for there is sodium fluoride, silica product in the method for traditional mode of production sodium fluoride product,
Have a rest operation, the high shortcoming of high labor intensive, consumption of raw materials and propose the present invention.
The content of the invention
In view of this, it is an object of the invention to propose a kind of method of continuous production sodium fluoride, the method production scale
Small investment, and Automated condtrol is capable of achieving, mitigating the labour intensity of employee, product quality is excellent, and consumption of raw materials is low.
Based on above-mentioned purpose, the method for a kind of continuous production sodium fluoride that the present invention is provided, is 20-30% by mass fraction
Sodium fluoride solution and mass fraction be continuously added in tubular reactor successively for the soda ash solution of 20-30%, control reaction
Temperature 60-100 DEG C, carries out metathesis reaction and generates sodium fluoride and silica slurry, and enter in continuously entering multistage floatation device
Row flotation, respectively obtains the slurry and silica containing slurry of containing sodium fluoride Jing after flotation, and Jing is centrifuged, washs, is dried respectively,
Sodium fluoride product and silica product are obtained；The solution that wherein each centrifugation is obtained is used as Recycling Mother Solution after merging.
In the present invention, it is preferred to, prodan is 1 with the mol ratio of soda ash：2.2-4；The time of metathesis reaction is
1-5 minutes；It is further preferred that prodan is 1 with the mol ratio of soda ash：2.5-3.
The present invention realizes the continuous production of sodium fluoride using the tubular reactor with spiral agitator and multistage floatation device.
In the present invention, it is preferred to, the tubular reactor is the tubular reactor with spiral agitator.
Prodan Method of Soda produces sodium fluoride, there is sodium fluoride and silica (white carbon) coprecipitation phenomena, easily
Formed " peritectoid ", this adds increased the separating difficulty of sodium fluoride and white carbon, also have impact on the quality of product.The present invention adopts fluorine
Sodium metasilicate is 1 with the mol ratio of soda ash：2.2-4, keeps soda ash to be reacted in excess conditions, and optimum mole ratio is 1：2.5-3,
Make pH more than 12, prodan is fully reacted, while it is existing to avoid the sodium fluoride for reacting generation peritectoid occur under high velocity agitation
As purity is high.
The present invention adopts the big excessive addition of soda ash, and prodan has obtained sufficient reaction during the course of the reaction, turns
Rate reaches 100%, and is not in peritectoid phenomenon, improves product quality.Excessive soda ash is recycled.
In the present invention, it is preferred to, solid soda ash is put in feed bin, dissolving tank is added with conveying worm, in dissolving
Mother liquor is continuously added in groove, under agitation with being steam heated to 60 DEG C -100 DEG C, dissolves soda ash, keep the soda ash after dissolving molten
The mass fraction of liquid is 20-30%, and is continuously extracted out in feeding tubular reactor with pump.In the process, control entering for mother liquor
Enter amount and the soda ash amount for adding, keep the concentration of the soda ash solution after dissolving.
In the present invention, it is further preferred that the speed of conveying worm is 1000kg/h, the addition flow of mother liquor is
3600-4000kg/h, with being steam heated to 75 DEG C -78 DEG C, the mass fraction of the soda ash solution after dissolving is 20-22%.
In the present invention, it is preferred to, solid prodan is put in feed bin, is added in pulping tank with conveying worm,
Mother liquor is continuously added in pulping tank, under agitation with being steam heated to 60 DEG C -100 DEG C, keeps the prodan after dissolving molten
The mass fraction of liquid is 20-30%, and is continuously extracted out in feeding tubular reactor with pump.In the process, control entering for mother liquor
Enter amount and the prodan amount for adding, keep the concentration of the sodium fluoride solution after dissolving.
In the present invention, it is further preferred that the water content of solid prodan is 6%, the speed of conveying worm is
900kg/h, the addition flow of mother liquor are 2400-2600kg/h, with being steam heated to 75 DEG C -78 DEG C, the prodan after dissolving
The mass fraction of solution is 25-27%.
In the present invention, it is preferred to, the flotation is comprised the following steps that：
(1) sodium fluoride and silica slurry are continuously entered in 1# floatation devices, flotation is entered by the reactant liquor of itself,
The slurry A of containing sodium fluoride is obtained from the bottom of floatation device, silica containing slurry a is obtained from top；
(2) the slurry A of containing sodium fluoride is sent in 2# floatation devices, flotation is carried out with mother liquor, fine silica is floatingly selected
Come, the slurry B of containing sodium fluoride is obtained from the bottom of floatation device, obtain silica containing slurry b from top；
(3) the slurry B of containing sodium fluoride is sent in 3# floatation devices, flotation and washing are carried out with soft water or industry water, from 3#
The bottom of floatation device obtains the slurry C of containing sodium fluoride, and the slurry c containing silica, soda ash is obtained from top；
(4) will send in 4# floatation devices after silica containing slurry a, slurry b merging, the slurry containing silica and soda ash
Flotation fluids of the material c as 4# floatation devices；The slurry C that thin sodium fluoride after flotation obtains containing sodium fluoride with 3# floatation devices bottom merges
After be sent from scheming and be centrifuged, obtain sodium fluoride product after drying；
(5) the silica containing slurry d from 4# floatation devices top out is sent from scheming and is centrifuged, after reusable heat water slurrying
It is centrifuged in being sent from scheming again, obtains silica product after drying.
In the present invention, the solution that each centrifugation in flotation step is obtained is used for front operation fluosilicic acid as mother liquor after merging
Sodium slurrying, the dissolving of soda ash, flotation fluid of floatation device etc., mother liquor are realized recycling；Each centrifugation includes three centrifugations, respectively
The slurry C that thin sodium fluoride in step (4) after flotation obtains containing sodium fluoride with 3# floatation devices bottom be sent from scheming after merging from
The heart, the silica containing slurry d in step (5) from 4# floatation devices top out are sent from scheming and are centrifuged, reusable heat water slurrying
It is centrifuged in being sent from scheming afterwards again.
In the present invention, it is preferred to, in step (2), mother liquor addition is 2000-3000kg/h；In step (3) soft water or
Industry water addition is 300-500kg/h.
In the present invention, it is preferred to, silica containing slurry d of the step (5) from 4# floatation devices top out is sent from the heart
Be centrifuged in machine, then with 70-100 DEG C of hot water slurrying after, heated with steam, 80 DEG C of keeping temperature, then be sent from scheming and be centrifuged, Jing
Silica product is obtained after 120 DEG C of dryings.
The acquisition of sodium fluoride product：Reacted slurry is continuously entered in 1# floatation devices, is entered by the reactant liquor of itself
Row flotation, obtains the slurry of containing sodium fluoride from bottom, obtains containing silica slurry from top, and the slurry of containing sodium fluoride is entered back into
In 2# floatation devices, flotation is carried out with mother liquor, be further separated out silica, carried out with soft water in then entering back into 3# floatation devices
After flotation and washing, Jing is centrifuged, is dried to obtain sodium fluoride product.Purity of Sodium Fluoride more than 98.5%, dioxide-containing silica is less than
0.4%, soda content is less than 0.2%, reaches primes standard.
The acquisition of silica product：By 1# floatation devices top obtain containing silica slurry with 2# floatation devices containing out
Silica slurry is combined into 4# floatation devices, carries out, after flotation, obtaining containing titanium dioxide from top with 3# tops liquid out
Silicon slurry, is sent from scheming and is centrifuged, and carries out thermosol with 70-100 DEG C of hot water again, is pressed from both sides with further reducing in silica
The soda ash of band, sodium fluoride, then Jing centrifugations, dry acquisition silica product.Silica purity more than 98.0%, sodium fluoride contains
Less than 0.8%, soda content is less than 1.0% to amount.
Compared with prior art, the method for the present invention has the advantages that：
(1) present invention realizes the continuous life of sodium fluoride using the tubular reactor with spiral agitator and multistage floatation device
Produce.The present invention using the big excessive addition of soda ash, makes prodan obtain sufficient reaction, conversion ratio during the course of the reaction
100% is reached, while avoiding the sodium fluoride for reacting generation peritectoid phenomenon occur under high velocity agitation, and multistage floatation device is adopted
Sodium fluoride and silica slurry to generating carries out flotation, improves product purity and quality.Given birth to using the method for the present invention
The Purity of Sodium Fluoride more than 98.5% of product, silica purity more than 98.0%.
(2) method of the present invention production scale small investment, and Automated condtrol is capable of achieving, mitigate the labour intensity of employee,
Product quality is excellent, and consumption of raw materials is low.In addition, in the method for continuous production sodium fluoride of the invention, mother liquor can be recycled, and enter
One step reduces production cost.
Description of the drawings
Accompanying drawing is, with reference to specific process embodiment, specifically to understand technique trend.
Fig. 1 is traditional production sodium fluoride technological process block-diagram；
Fig. 2 is the continuous production sodium fluoride technological process block-diagram of the present invention.
Specific embodiment
To make the object, technical solutions and advantages of the present invention become more apparent, below in conjunction with specific embodiment, and reference
Accompanying drawing, the present invention is described in more detail.
Embodiment 1
The present embodiment continuously produces the technological process block-diagram of sodium fluoride as shown in Fig. 2 comprising the following steps that：
(1) solid soda ash is put in feed bin, the speed for pressing 1000kg/h with conveying worm adds dissolving tank, in dissolving
It is continuously added to the mother liquor of rear operation in groove, adds flow 3600-4000kg/h, under agitation with being steam heated to 75 DEG C -78 DEG C,
Dissolve soda ash, the concentration (mass fraction) of the soda ash solution after dissolving is kept in 20-22%, and continuously extract feeding pipe out with pump
In formula reactor；
(2) solid prodan (water content 6%) is put in feed bin, is added by the speed of 900kg/h with conveying worm
Enter in pulping tank, the mother liquor of operation after being continuously added in pulping tank, add flow 2400-2600kg/h, under agitation with steaming
Vapour is heated to 75 DEG C -78 DEG C, and the solid-to-liquid ratio (mass fraction of prodan) in holding prodan slurry is 25-27%, and
Continuously extracted out in feeding tubular reactor with pump；
(3) spiral agitator in tubular reactor, controlling reaction temperature 80-85 DEG C, soda ash solution and fluorine silicon are started
Acid sodium solution carries out metathesis reaction, generate sodium fluoride and silica slurry, and control material (prodan and soda ash) rubs
You compare 1：2.2-4 (pH is more than 12), minute in reaction time 1-5；
(4) reacted sodium fluoride and silica slurry are entered in 1# floatation devices, is entered by the reactant liquor of itself
Flotation, obtains the slurry A of containing sodium fluoride from the bottom of floatation device, obtains silica containing slurry a from top；
(5) the slurry A of containing sodium fluoride being sent in 2# floatation devices, flotation being carried out with the centrifuge mother liquor of rear operation, mother liquor adds
Enter amount 2000kg/h, fine silica flotated by flotation, the slurry B of containing sodium fluoride is obtained from the bottom of floatation device,
Silica containing slurry b is obtained from top；
(6) the slurry B of containing sodium fluoride is sent in 3# floatation devices, flotation and washing, soft water are carried out with soft water or industry water
Or industry water addition 300kg/h, obtain the slurry C of containing sodium fluoride from the bottom of floatation device, from top obtain containing silica,
The slurry c of soda ash etc.；
(7) send into after silica containing slurry a, slurry b merge in 4# floatation devices, the slurry containing silica and soda ash etc.
Flotation fluids of the material c as 4# floatation devices；The slurry C that thin sodium fluoride after flotation obtains containing sodium fluoride with 3# floatation devices bottom merges
After be sent from scheming and be centrifuged, obtain sodium fluoride product after drying, weight 1120kg analyzes Purity of Sodium Fluoride therein
98.5%, dioxide-containing silica is less than 0.4%, and soda content is less than 0.2%, reaches primes standard；
(8) the silica containing slurry d from 4# floatation devices top out is sent from scheming and is centrifuged, then with 70-100 DEG C
After hot water slurrying, heated with steam, 80 DEG C of keeping temperature, then be centrifuged in being sent from scheming, silica is obtained Jing after 120 DEG C of dryings
(white carbon) product, weight 450kg (containing water is combined), silica purity more than 98.0%, fluorination sodium content are less than 0.8%,
Soda content is less than 1.0%；
(9) solution that each centrifugation (the once centrifugation in step (7), the centrifugation twice in step (8)) obtains is made after merging
It is used for front process (2) prodan slurrying, the dissolving of step (1) soda ash, the flotation fluid of step (5) 2# floatation devices for mother liquor
Deng mother liquor realization recycling.
Embodiment 2
The present embodiment continuously produces the technological process block-diagram of sodium fluoride as shown in Fig. 2 comprising the following steps that：
(1) solid soda ash is put in feed bin, the speed for pressing 1000kg/h with conveying worm adds dissolving tank, in dissolving
It is continuously added to the mother liquor of rear operation in groove, adds flow 3600-4000kg/h, under agitation with being steam heated to 80 DEG C -85 DEG C,
Dissolve soda ash, the concentration (mass fraction) of the soda ash solution after dissolving is kept in 26-28%, and continuously extract feeding pipe out with pump
In formula reactor；
(2) solid prodan (water content 6%) is put in feed bin, is added by the speed of 900kg/h with conveying worm
Enter in pulping tank, the mother liquor of operation after being continuously added in pulping tank, add flow 2400-2600kg/h, under agitation with steaming
Vapour is heated to 80 DEG C -85 DEG C, and the solid-to-liquid ratio (mass fraction of prodan) in holding prodan slurry is 22-25%, and
Continuously extracted out in feeding tubular reactor with pump；
(3) spiral agitator in tubular reactor, controlling reaction temperature 88-90 DEG C, soda ash solution and fluorine silicon are started
Acid sodium solution carries out metathesis reaction, generate sodium fluoride and silica slurry, and control material (prodan and soda ash) rubs
You compare 1：2.5-3 (pH is more than 12), minute in reaction time 1-5；
(4) reacted sodium fluoride and silica slurry are entered in 1# floatation devices, is entered by the reactant liquor of itself
Flotation, obtains the slurry A of containing sodium fluoride from the bottom of floatation device, obtains silica containing slurry a from top；
(5) the slurry A of containing sodium fluoride being sent in 2# floatation devices, flotation being carried out with the centrifuge mother liquor of rear operation, mother liquor adds
Enter amount 3000kg/h, fine silica flotated by flotation, the slurry B of containing sodium fluoride is obtained from the bottom of floatation device,
Silica containing slurry b is obtained from top；
(6) the slurry B of containing sodium fluoride is sent in 3# floatation devices, flotation and washing, soft water are carried out with soft water or industry water
Or industry water addition 500kg/h, obtain the slurry C of containing sodium fluoride from the bottom of floatation device, from top obtain containing silica,
The slurry c of soda ash etc.；
(7) send into after silica containing slurry a, slurry b merge in 4# floatation devices, the slurry containing silica and soda ash etc.
Flotation fluids of the material c as 4# floatation devices；The slurry C that thin sodium fluoride after flotation obtains containing sodium fluoride with 3# floatation devices bottom merges
After be sent from scheming and be centrifuged, obtain sodium fluoride product after drying, weight 1100kg analyzes Purity of Sodium Fluoride therein
98.8%, dioxide-containing silica is less than 0.3%, and soda content is less than 0.2%, reaches primes standard；
(8) the silica containing slurry d from 4# floatation devices top out is sent from scheming and is centrifuged, then with 70-100 DEG C
After hot water slurrying, heated with steam, 80 DEG C of keeping temperature, then be centrifuged in being sent from scheming, silica is obtained Jing after 120 DEG C of dryings
(white carbon) product, weight 430kg (containing water is combined), silica purity more than 98.1%, fluorination sodium content are less than 0.7%,
Soda content is less than 1.0%；
(9) solution that each centrifugation (the once centrifugation in step (7), the centrifugation twice in step (8)) obtains is made after merging
It is used for front process (2) prodan slurrying, the dissolving of step (1) soda ash, the flotation fluid of step (5) 2# floatation devices for mother liquor
Deng mother liquor realization recycling.
Embodiment 3
The present embodiment continuously produces the technological process block-diagram of sodium fluoride as shown in Fig. 2 comprising the following steps that：
(1) solid soda ash is put in feed bin, the speed for pressing 1000kg/h with conveying worm adds dissolving tank, in dissolving
It is continuously added to the mother liquor of rear operation in groove, adds flow 3600-4000kg/h, under agitation with being steam heated to 60 DEG C -65 DEG C,
Dissolve soda ash, the concentration (mass fraction) of the soda ash solution after dissolving is kept in 23-25%, and continuously extract feeding pipe out with pump
In formula reactor；
(2) solid prodan (water content 6%) is put in feed bin, is added by the speed of 900kg/h with conveying worm
Enter in pulping tank, the mother liquor of operation after being continuously added in pulping tank, add flow 2400-2600kg/h, under agitation with steaming
Vapour is heated to 60 DEG C -65 DEG C, and the solid-to-liquid ratio (mass fraction of prodan) in holding prodan slurry is 28-30%, and
Continuously extracted out in feeding tubular reactor with pump；
(3) spiral agitator in tubular reactor, controlling reaction temperature 68-70 DEG C, soda ash solution and fluorine silicon are started
Acid sodium solution carries out metathesis reaction, generate sodium fluoride and silica slurry, and control material (prodan and soda ash) rubs
You compare 1：3-4 (pH is more than 12), minute in reaction time 1-5；
(4) reacted sodium fluoride and silica slurry are entered in 1# floatation devices, is entered by the reactant liquor of itself
Flotation, obtains the slurry A of containing sodium fluoride from the bottom of floatation device, obtains silica containing slurry a from top；
(5) the slurry A of containing sodium fluoride being sent in 2# floatation devices, flotation being carried out with the centrifuge mother liquor of rear operation, mother liquor adds
Enter amount 2500kg/h, fine silica flotated by flotation, the slurry B of containing sodium fluoride is obtained from the bottom of floatation device,
Silica containing slurry b is obtained from top；
(6) the slurry B of containing sodium fluoride is sent in 3# floatation devices, flotation and washing, soft water are carried out with soft water or industry water
Or industry water addition 400kg/h, obtain the slurry C of containing sodium fluoride from the bottom of floatation device, from top obtain containing silica,
The slurry c of soda ash etc.；
(7) send into after silica containing slurry a, slurry b merge in 4# floatation devices, the slurry containing silica and soda ash etc.
Flotation fluids of the material c as 4# floatation devices；The slurry C that thin sodium fluoride after flotation obtains containing sodium fluoride with 3# floatation devices bottom merges
After be sent from scheming and be centrifuged, obtain sodium fluoride product after drying, weight 1130kg analyzes Purity of Sodium Fluoride therein
98.7%, dioxide-containing silica is less than 0.4%, and soda content is less than 0.2%, reaches primes standard；
(8) the silica containing slurry d from 4# floatation devices top out is sent from scheming and is centrifuged, then with 70-100 DEG C
After hot water slurrying, heated with steam, 80 DEG C of keeping temperature, then be centrifuged in being sent from scheming, silica is obtained Jing after 120 DEG C of dryings
(white carbon) product, weight 460kg (containing water is combined), silica purity more than 98.3%, fluorination sodium content are less than 0.8%,
Soda content is less than 1.0%；
(9) solution that each centrifugation (the once centrifugation in step (7), the centrifugation twice in step (8)) obtains is made after merging
It is used for front process (2) prodan slurrying, the dissolving of step (1) soda ash, the flotation fluid of step (5) 2# floatation devices for mother liquor
Deng mother liquor realization recycling.
Comparative example 1
This comparative example produces sodium fluoride technological process block-diagram as shown in figure 1, comprising the following steps that：
(1) solid soda ash will be put under agitation in mother liquor or water input dissolving tank, after heating for dissolving, proceed to head tank,
Concentration 20-22% soda ash solution；
(2) solid prodan (water content 6%) will be put under agitation in mother liquor or water input pulping tank, be prepared as containing
Gu amount is the prodan slurry of 20-30%, proceed in reactor；
(3) start reactor agitator, be heated to 60-80 DEG C, soda ash solution is gradually added, pH7.5-8 is controlled for eventually
Point (control mol ratio 1：2) will be rinsed with mother liquor in, being put into washbasin；
(4) again the sodium fluoride in washbasin is centrifuged with manually shoveling into centrifuge, is dried and obtains sodium fluoride product, weight
Amount 1000kg, analyzes Purity of Sodium Fluoride 95.0% therein, and dioxide-containing silica is less than 2.0%, and soda content is less than 1.0%；
(5) silica for rinsing out is sent from scheming and is centrifuged out silica, obtain two after drying
Silica (white carbon) product, weight 400kg (containing water is combined), silica purity more than 85.0%, fluorination sodium content are less than
1.8%, soda content is less than 1.5%.
This comparative example is identical with the solid prodan of embodiment 1-3 (water content 6%) and the input amount of solid soda ash.
The present invention can be seen that by the comparing result of embodiment 1-3 and comparative example 1 anti-using the tubular type with spiral agitator
Device and multistage floatation device is answered to realize sodium fluoride continuous prodution and operation, the mother liquor in production process can be recycled, and enter
One step reduces production cost；And prodan has obtained sufficient reaction, conversion ratio reaches 100%, significantly larger than contrasts
The conversion ratio (90%) of prodan in example 1；While the Purity of Sodium Fluoride more than 98.5% of embodiment 1-3 kind, silica is pure
Degree more than 98.0%, also significantly larger than in comparative example 1 sodium fluoride and silica purity.Therefore, the continuous production fluorine of the present invention
Change the method for sodium no matter from production technology, or from the point of view of the purity of the conversion ratio of raw material, product, better than in comparative example 1
Method.
In sum, the present invention realizes sodium fluoride using the tubular reactor with spiral agitator and multistage floatation device
It is continuous to produce.The present invention using the big excessive addition of soda ash, makes prodan obtain sufficient reaction during the course of the reaction,
Conversion ratio reaches 100%, while avoid the sodium fluoride for reacting generation peritectoid phenomenon occur under high velocity agitation, and using multistage
Floatation device carries out flotation to the sodium fluoride and silica slurry of generation, improves product purity and quality.Using the present invention's
The Purity of Sodium Fluoride more than 98.5% of method production, silica purity more than 98.0%.Method of the present invention production scale is thrown
Money is few, and is capable of achieving Automated condtrol, mitigates the labour intensity of employee, and product quality is excellent, and consumption of raw materials is low.In addition, at this
In bright continuous production sodium fluoride method, mother liquor can be recycled, and reduce further production cost.
Those of ordinary skill in the art should be understood：The discussion of any of the above embodiment is exemplary only, not
It is intended to imply that the scope of the present disclosure (including claim) is limited to these examples；Under the thinking of the present invention, above example
Or can also be combined between the technical characteristic in different embodiments, and there is the different aspect of the present invention as above
Many other changes, in order to it is simple and clear they provide without in details.Therefore, it is all within the spirit and principles in the present invention,
Any omission for being made, modification, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (10)
1. it is a kind of it is continuous production sodium fluoride method, it is characterised in that by mass fraction for 20-30% sodium fluoride solution and
Mass fraction is continuously added in tubular reactor successively for the soda ash solution of 20-30%, and controlling reaction temperature 60-100 DEG C is carried out
Metathesis reaction generates sodium fluoride and silica slurry, and carries out flotation in continuously entering multistage floatation device, divides Jing after flotation
The slurry and silica containing slurry of containing sodium fluoride are not obtained, Jing is centrifuged, washs, is dried respectively, that is, obtain sodium fluoride product
And silica product；The solution that wherein each centrifugation is obtained is used as Recycling Mother Solution after merging.
2. the method for continuous production sodium fluoride according to claim 1, it is characterised in that prodan and soda ash mole
Than for 1：2.2-4；The time of metathesis reaction is 1-5 minutes；The tubular reactor is that the tubular type with spiral agitator is anti-
Answer device.
3. the method for continuous production sodium fluoride according to claim 2, it is characterised in that prodan and soda ash mole
Than for 1：2.5-3.
4. it is according to claim 1 it is continuous production sodium fluoride method, it is characterised in that solid soda ash is put into into feed bin
In, dissolving tank is added with conveying worm, mother liquor is continuously added in dissolving tank, under agitation with being steam heated to 60 DEG C -100
DEG C, dissolve soda ash, the mass fraction for keeping the soda ash solution after dissolving is 20-30%, and continuously extracts feeding tubular type out with pump
In reactor.
5. the method for continuous production sodium fluoride according to claim 4, it is characterised in that the speed of conveying worm is
1000kg/h, the addition flow of mother liquor are 3600-4000kg/h, with being steam heated to 75 DEG C -78 DEG C, the soda ash solution after dissolving
Mass fraction be 20-22%.
6. it is according to claim 1 it is continuous production sodium fluoride method, it is characterised in that by solid prodan input expect
In storehouse, added in pulping tank with conveying worm, mother liquor is continuously added in pulping tank, under agitation with being steam heated to 60
DEG C -100 DEG C, the mass fraction for keeping the sodium fluoride solution after dissolving is 20-30%, and it is anti-continuously to extract feeding tubular type out with pump
In answering device.
7. it is according to claim 6 it is continuous production sodium fluoride method, it is characterised in that the water content of solid prodan
For 6%, the speed of conveying worm is 900kg/h, and the addition flow of mother liquor is 2400-2600kg/h, with being steam heated to 75
DEG C -78 DEG C, the mass fraction of the sodium fluoride solution after dissolving is 25-27%.
8. it is according to claim 1 it is continuous production sodium fluoride method, it is characterised in that the concrete steps of the flotation are such as
Under：
(1) sodium fluoride and silica slurry are continuously entered in 1# floatation devices, flotation is entered by the reactant liquor of itself, from floating
Select the bottom of device to obtain the slurry A of containing sodium fluoride, silica containing slurry a is obtained from top；
(2) the slurry A of containing sodium fluoride is sent in 2# floatation devices, flotation is carried out with mother liquor, fine silica is flotated, from
The bottom of floatation device obtains the slurry B of containing sodium fluoride, obtains silica containing slurry b from top；
(3) the slurry B of containing sodium fluoride is sent in 3# floatation devices, flotation and washing are carried out with soft water or industry water, from 3# flotation
The bottom of device obtains the slurry C of containing sodium fluoride, and the slurry c containing silica, soda ash is obtained from top；
(4) will send in 4# floatation devices after silica containing slurry a, slurry b merging, the slurry c containing silica and soda ash
As the flotation fluid of 4# floatation devices；After the slurry C that thin sodium fluoride after flotation obtains containing sodium fluoride with 3# floatation devices bottom merges
It is centrifuged in being sent from scheming, obtains sodium fluoride product after drying；
(5) the silica containing slurry d from 4# floatation devices top out is sent from scheming and is centrifuged, and is sent after reusable heat water slurrying again
It is centrifuged in centrifuge, obtains silica product after drying.
9. it is according to claim 8 it is continuous production sodium fluoride method, it is characterised in that mother liquor addition in step (2)
For 2000-3000kg/h；In step (3), soft water or industry water addition are 300-500kg/h.
10. it is according to claim 8 it is continuous production sodium fluoride method, it is characterised in that step (5) is from 4# floatation devices
Portion silica containing slurry d out is sent from scheming and is centrifuged, then with 70-100 DEG C of hot water slurrying after, heated with steam,
80 DEG C of keeping temperature, then be centrifuged in being sent from scheming, silica product is obtained Jing after 120 DEG C of dryings.
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| CN110606492A (en) * | 2019-10-29 | 2019-12-24 | 朱志宏 | Method for continuously synthesizing white carbon black and sodium fluoride |
| CN115594198A (en) * | 2022-10-20 | 2023-01-13 | 山东海科创新研究院有限公司（Cn） | Method for preparing battery-grade sodium fluoride by one-step method and obtained product |
| CN117361570A (en) * | 2023-09-12 | 2024-01-09 | 山东立中新能源材料有限公司 | Method for preparing battery grade sodium fluoride from sodium carbonate and sodium fluosilicate |
| CN117446833A (en) * | 2023-09-20 | 2024-01-26 | 山东立中新能源材料有限公司 | Preparation method of sodium hexafluorophosphate for sodium battery |
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| CN115594198A (en) * | 2022-10-20 | 2023-01-13 | 山东海科创新研究院有限公司（Cn） | Method for preparing battery-grade sodium fluoride by one-step method and obtained product |
| CN117361570A (en) * | 2023-09-12 | 2024-01-09 | 山东立中新能源材料有限公司 | Method for preparing battery grade sodium fluoride from sodium carbonate and sodium fluosilicate |
| CN117361570B (en) * | 2023-09-12 | 2024-05-14 | 山东立中新能源材料有限公司 | Method for preparing battery grade sodium fluoride from sodium carbonate and sodium fluosilicate |
| CN117446833A (en) * | 2023-09-20 | 2024-01-26 | 山东立中新能源材料有限公司 | Preparation method of sodium hexafluorophosphate for sodium battery |
| CN117446833B (en) * | 2023-09-20 | 2024-05-14 | 山东立中新能源材料有限公司 | Preparation method of sodium hexafluorophosphate for sodium battery |
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