CN108793192A - A kind of preparation method and its preparation system of ammonium fluoride - Google Patents
A kind of preparation method and its preparation system of ammonium fluoride Download PDFInfo
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- CN108793192A CN108793192A CN201810948368.9A CN201810948368A CN108793192A CN 108793192 A CN108793192 A CN 108793192A CN 201810948368 A CN201810948368 A CN 201810948368A CN 108793192 A CN108793192 A CN 108793192A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/162—Ammonium fluoride
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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 present invention relates to a kind of preparation method of ammonium fluoride and its preparation systems, including ammonia tank, fluorination hydrogen gas tank, anhydrous organic solvent tank, reaction kettle, centrifuge, mother liquor tank, condensing unit, thermometer and pH meter, ammonia and hydrogen fluoride are dissolved in organic solvent successively, hydrogen fluoride reacts the anhydrous ammonium fluoride of production with ammonia in the organic solvent；The hydrogen fluoride is higher than solubility of the anhydrous ammonium fluoride in the organic solvent with solubility of the ammonia in the organic solvent.Anhydrous ammonium fluoride powder size that the preparation method obtains is small, purity is high, and organic solvent can recycle always in reaction.
Description
Technical field
The present invention relates to chemical field, more particularly to the preparation method and its preparation system of a kind of ammonium fluoride.
Background technology
Production method difference vapor phase method, sublimed method and the liquid phase method of ammonium fluoride.It is industrial commonly in liquid phase method
And method：In lead system or plastic containers, quantitative hydrofluoric acid is put into.In container external application water cooling, it is slowly introducing ammonia under stiring,
Until reaction solution Ph values up to until 4 or so.Ammonium fluoride product is made through crystallisation by cooling, centrifugation, pneumatic conveying drying in reaction solution.
Reaction principle is as follows：NH3+HF→NH4F.But there are some defects for the method, for example, in legal preparation ammonium fluoride water content it is high, pure
Bottom is spent, and is discharged into the ammonia in air and hydrogen fluoride gas is more, environmental pollution is larger.In addition, the ammonium fluoride acid of method production
Spend uneven, the content of metal impurities is higher.
Invention content
For this reason, it may be necessary to provide a kind of easy to operate, safe operation process, pollution, the lower fluorination of production cost are not generated
Ammonium preparation method and its mating preparation system.
A kind of preparation method of ammonium fluoride is inventor provided, ammonia and hydrogen fluoride are dissolved in organic solvent successively, fluorine
Change hydrogen and reacts the anhydrous ammonium fluoride of production in the organic solvent with ammonia；
The hydrogen fluoride is higher than the anhydrous ammonium fluoride described organic molten with solubility of the ammonia in the organic solvent
Solubility in agent.
Further, the hydrogen fluoride and solubility of the ammonia in the organic solvent are in 20g or more, the anhydrous fluorination
Solubility of the ammonium in the organic solvent is in 1g or less.
Further, the organic solvent includes or mixtures thereof methanol, ethyl alcohol, acetonitrile, dichloromethane.
Further, the preparation method comprises the following steps：
Ammonia solution is prepared：Liquefied ammonia is incorporated in the organic solvent, is uniformly mixed, ammonia solution is configured；
Ammonium fluoride synthesizes：Hydrogen fluoride gas is passed through into ammonia solution, hydrogen fluoride is reacted with ammonia solution generates anhydrous fluorination
Ammonium, white anhydrous ammonium fluoride powder are precipitated from reaction solution.
Further, in the ammonia solution preparation steps, the mass ratio of the liquefied ammonia and the organic solvent is 5-50:
50-95。
Further, in the ammonium fluoride synthesis step, the pH value for being passed through hydrogen fluoride gas to reaction solution is whole after 7-8
Only react.
When the mass ratio of ammonia and organic solvent is 50:When 50, the pH value of reaction terminating is 8；And when ammonia and organic solvent
Mass ratio is 5:When 95, the pH value of reaction terminating is 7.
Further, in the ammonia solution preparation steps, the addition speed of the liquefied ammonia is 10L/min-500L/min；Institute
It states in ammonium fluoride synthesis step, the draft speed of hydrogen fluoride is 10L/min-500L/min.
Further, in the ammonia solution preparation steps, feed temperature control is at 10 DEG C -30 DEG C, ammonia solution final temperature
Control is at 0 DEG C -10 DEG C.In the ammonium fluoride synthesis step, reaction temperature is controlled at 10 DEG C -30 DEG C, avoids pyroreaction excessively
Acutely.
Control ammonia solution temperature is gradually reduced to 0 DEG C -10 DEG C, and ammonia solution is configured to highly exothermic reaction, is carried out to temperature
Control can reduce the severe degree of reaction, enhance the safety of operation.Meanwhile the temperature of ammonia solution is finally reduced to 0 DEG C -10
DEG C, contribute to the control of temperature in later stage ammonium fluoride synthesis step, controlling reaction temperature to avoid reaction excessively violent.
Further, the preparation method further includes solid-liquid separation step and vacuum drying step, the specific steps are：
It is separated by solid-liquid separation：The solution containing white anhydrous ammonium fluoride powder that ammonium fluoride synthesis step obtains is subjected to solid-liquid point
From obtaining ammonium fluoride crude product,
Vacuum drying：Ammonium fluoride crude product is subjected to reduced vacuum drying, obtains fluorination ammonium product.
Inventor additionally provides a kind of system preparing ammonium fluoride, including without ammonia tank, fluorination hydrogen gas tank, anhydrous organic molten
Agent tank, reaction kettle, centrifuge, mother liquor tank, condensing unit, thermometer and pH meter；
The reaction kettle bottom of chamber is provided with blender, and liquefied ammonia inlet, hydrogen fluoride air inlet are offered above the reaction kettle
Mouth, anhydrous organic solvent inlet, exhaust outlet, the first refluxing opening, the second refluxing opening, thermometer mouth and pH meter mouth, it is described anti-
Answer and offer reaction kettle liquid outlet below kettle, the ammonia tank liquid outlet by the liquefied ammonia that is opened up on the first valve and reaction kettle into
Liquid mouth is connected, and the fluorination hydrogen gas tank gas outlet is connected by the second valve with the hydrogen fluoride air inlet opened up on reaction kettle
Logical, the anhydrous organic solvent tank liquid outlet is connected by third valve with the anhydrous organic solvent inlet opened up on reaction kettle
Logical, the reaction kettle liquid outlet is connected by centrifuge and the 4th valve with the mother liquor tank inlet opened up on mother liquor tank,
The mother liquor tank liquid outlet opened up on the mother liquor tank is connected by delivery pump with the first refluxing opening, and the thermometer passes through temperature
Meter mouth plugs in a kettle, and the pH meter is plugged in a kettle by pH meter mouth；
The condensing unit includes condenser, gas-liquid separator and dump tank, the exhaust outlet by condenser and
5th valve is connected with the gas-liquid separator inlet that gas-liquid separator upper end opens up, and the gas-liquid separator lower end offers
The first liquid outlet of gas-liquid separator offers the second liquid outlet of gas-liquid separator, the dump tank on the side of gas-liquid separator
Upper end offers dump tank inlet, and the first liquid outlet of the gas-liquid separator is connected by the 6th valve with dump tank inlet
Logical, the second liquid outlet of the gas-liquid separator is connected by the 7th valve with the second refluxing opening；
The reaction kettle cavity wall is sandwich, offers coolant liquid inlet and cold in the reaction kettle cavity wall respectively
But liquid liquid outlet, coolant liquid inlet external refrigerant source are provided with the 8th valve at the coolant liquid inlet.
It being different from the prior art, above-mentioned technical proposal provides a kind of preparation method and its preparation system of ammonium fluoride, according to
It is secondary by ammonia and hydrofluoric acid dissolution in organic solvent, ammonia reacts in organic solvent with hydrofluoric acid produces anhydrous ammonium fluoride；It is described
Hydrogen fluoride is higher than solubility of the anhydrous ammonium fluoride in the organic solvent with solubility of the ammonia in the organic solvent.
Anhydrous ammonium hydrogen fluoride powder size that the preparation method obtains is small, purity is high, and organic solvent can recycle always in reaction.
Description of the drawings
Fig. 1 is a kind of structural schematic diagram for the equipment preparing ammonium fluoride of the present embodiment.
Reference sign：
1, ammonia tank；
2, it is fluorinated hydrogen tank；
3, anhydrous organic solvent tank；
4, reaction kettle；
41, thermometer；
42, pH meter；
43, blender；
44, reaction kettle cavity wall；
441, coolant liquid inlet；
442, coolant liquid liquid outlet；
5, centrifuge；
6, mother liquor tank；
71, condenser；
72, gas-liquid separator；
73, dump tank；
81, the first valve；
82, the second valve；
83, third valve；
84, the 4th valve；
85, the 5th valve；
86, the 6th valve；
87, the 7th valve.
Specific implementation mode
For the technology contents of technical solution, construction feature, the objects and the effects are described in detail, below in conjunction with specific reality
It applies example and Figure of description 1 is coordinated to be explained in detail.
The preparation of 1 ammonium fluoride of embodiment
Referring to Fig. 1, inventor providing a kind of system preparing ammonium fluoride, system includes ammonia tank 1, fluorination hydrogen gas tank
2, anhydrous organic solvent tank 3, reaction kettle 4 and centrifuge 5, mother liquor tank 6, condensing unit, thermometer 41 and pH meter 42；
Ammonia tank prepares the raw materials ammonia of ammonium fluoride for splendid attire, and fluorination hydrogen gas tank prepares the raw material of ammonium fluoride for splendid attire
Hydrogen fluoride gas, anhydrous organic solvent tank is for containing anhydrous organic solvent, and ammonium fluoride is in anhydrous organic solvent by ammonia and nothing
Water hydrogen fluoride reaction generates, the container that reaction kettle is reacted as ammonium fluoride, and the effect of centrifuge is will to react the ammonium fluoride generated
It is separated from the solution in reaction kettle, to obtain ammonium fluoride product, mother liquor tank is centrifuged for containing from centrifuge
The solution isolated, and be conveyed back in reaction kettle and continue to participate in reaction.
The reaction kettle bottom of chamber is provided with blender 43, and the blender is generated for mixing liquefied ammonia with anhydrous organic solvent
Ammonia solution, blender can be used for mixing ammonia solution and be fluorinated hydrogen during being passed through hydrogen fluoride gas into reaction kettle
Body further includes actuating unit, and blender is sequentially connected with actuating unit, and actuating unit drives blender to rotate in a kettle and stirs
Liquefied ammonia, anhydrous organic solvent, anhydrous hydrogen fluoride are mixed, its is made more uniform to be distributed in reaction kettle so that reaction is uniformly happened at
In the organic solvent of reaction kettle, hot-spot phenomenon caused by avoiding local concentration excessive, while reaction being contributed to radiate.
Liquefied ammonia inlet, hydrogen fluoride air inlet, anhydrous organic solvent inlet, exhaust are offered above the reaction kettle
Mouth, the first refluxing opening, the second refluxing opening and thermometer mouth and pH meter mouth, liquefied ammonia inlet is for inputting liquid into reaction kettle
Ammonia, hydrogen fluoride air inlet are used for for inputting hydrogen fluoride gas, anhydrous organic solvent inlet into reaction kettle into reaction kettle
Anhydrous organic solvent is inputted, it is exothermic reaction to prepare ammonium fluoride in reaction kettle, gas meeting during reaction in reaction kettle
Expansion, exhaust outlet is used to avoid feeling suffocated in reaction kettle by the expanding gas output-response kettle in reaction kettle and the feelings exploded
Condition, the effect of the first refluxing opening are inputted back what is contained in mother liquor tank in reaction kettle by the solution that centrifuge is isolated,
The effect of second refluxing opening is that the ammonia that will be isolated in gas-liquid separator is transmitted back in reaction kettle with hydrogen fluoride gas and continues to join
Add reaction.Reaction kettle liquid outlet is offered below the reaction kettle, the effect of reaction kettle liquid outlet is will fluorination after the completion of reacting
Liquid output-response kettle in ammonium product and kettle.
The ammonia tank liquid outlet is connected by the first valve 81 and pipeline with the liquefied ammonia inlet opened up on reaction kettle
Logical, the fluorination hydrogen gas tank gas outlet is connected by the second valve 82 and pipeline with the hydrogen fluoride air inlet opened up on reaction kettle
Logical, the anhydrous organic solvent tank liquid outlet passes through the anhydrous organic solvent that is opened up on third valve 83 and pipeline and reaction kettle
Inlet is connected, the reaction kettle liquid outlet by the mother liquor tank that is opened up on centrifuge and the 4th valve 84 and mother liquor tank into
Liquid mouth is connected, and the mother liquor tank liquid outlet opened up on the mother liquor tank is connected by delivery pump with the first refluxing opening.
The first valve and third valve are opened, the liquefied ammonia in ammonia tank is input in reaction kettle, anhydrous organic solvent tank
In anhydrous organic solvent be input in reaction kettle, and start blender, uniformly mix liquefied ammonia and anhydrous organic solvent, then open
Second valve is passed through hydrogen fluoride gas into reaction kettle, and ammonium fluoride is finally made, and opens the 4th valve, the fluorination in reaction kettle
Ammonium product and the remaining solution of reaction are input in centrifuge, and centrifuge isolates ammonium fluoride product from solution, remaining
Solution be transported in mother liquor tank, then open delivery pump, the solution in mother liquor tank be transported to reaction kettle by the first refluxing opening
In.
The condensing unit includes condenser 71, gas-liquid separator 72 and dump tank 73, and the effect of condenser is cooling
The main component of the gas exported from exhaust outlet, the gas of discharge is ammonia, also a small amount of hydrogen fluoride gas and vaporization
Organic solvent.The effect of gas-liquid separator is for detaching, realizing from gas by the organic solvent condensed in condenser
The purpose of gas-liquid separation, and the organic solvent for being condensed into liquid is stored in dump tank, remaining ammonia and fluorination hydrogen
Body, which is passed through in reaction kettle, to be continued to participate in reaction.
The gas-liquid separation that the exhaust outlet is opened up by condenser, the 5th valve 85 and pipeline and gas-liquid separator upper end
Device inlet is connected, and the gas-liquid separator lower end offers the first liquid outlet of gas-liquid separator, the side of gas-liquid separator
On offer the second liquid outlet of gas-liquid separator, the dump tank upper end offers dump tank inlet, the gas-liquid separator
First liquid outlet is connected by the 6th valve 86 with dump tank inlet, and the second liquid outlet of the gas-liquid separator passes through the 7th
Valve 87 is connected with the second refluxing opening.
It is inputted in condenser by pipeline because of the gas of expanded by heating in reaction kettle, starts condenser, it will be in condenser
Steam state organic solvent condensate opens the 5th valve at liquid, and the organic solvent for being condensed into liquid carries ammonia and hydrogen fluoride gas
It being transported in gas-liquid separator from condenser, gas-liquid separator isolates ammonia with hydrogen fluoride gas from organic solvent,
The 6th valve is opened, the organic solvent in gas-liquid separator is transported in dump tank, then opens the 7th valve, in gas-liquid separator
Ammonia and hydrogen fluoride gas be transmitted back in reaction kettle by the second refluxing opening.In certain preferred embodiments, the gas-liquid
It is equipped with blow valve at separator inlet, avoids condensing unit there is a phenomenon where feeling suffocated, is mainly discharged from condensing unit
Gas is air, and main component is nitrogen.
The reaction kettle cavity wall 44 is sandwich, i.e. reaction kettle cavity wall is divided into inner wall and outer wall, by inner wall and outer wall it
Between the interlayer that constitutes be coolant liquid the flowing space, offer respectively in the reaction kettle cavity wall coolant liquid inlet 441 and
Coolant liquid liquid outlet 442, coolant liquid inlet and coolant liquid liquid outlet are the through-hole structures run through by outer wall in interlayer,
Coolant liquid inlet external refrigerant source is provided with the 8th valve at the coolant liquid inlet, and refrigerant source passes through coolant liquid feed liquor
Mouth injects coolant liquid into the interlayer of reaction kettle, and coolant liquid is flowed from coolant liquid inlet in interlayer, and goes out liquid from coolant liquid
Mouth outflow interlayer, to reduce the temperature in reaction kettle.In certain preferred embodiments, the coolant liquid inlet is opened in instead
The lower section of kettle, coolant liquid liquid outlet is answered to be opened in the top of reaction kettle, advantage is that it is possible to so that coolant liquid filling is full
The interlayer of reaction kettle, cooling effect is more preferably；
In certain preferred embodiments, when needing to overhaul reaction kettle, external air at coolant liquid liquid outlet,
It is passed through air into the interlayer cavity wall of reaction kettle, will be overhauled after the refrigerant emptying in sandwich.
In certain preferred embodiments, the coolant liquid is brine, and advantage is：Fusing point of the brine compared with clear water
It reduces, more heats can be absorbed, and cost is relatively low for other coolant liquids.
The thermometer is used to monitor in real time the reaction temperature in reaction kettle, and thermometer is offered above the reaction kettle
Mouthful, the thermometer is plugged in thermometer mouth.
The pH meter is used to monitor in real time the pH value in reaction kettle, and pH meter mouth, the pH are offered above the reaction kettle
Meter is plugged in pH meter mouth.
In certain preferred embodiments, the coolant liquid is brine, and advantage is：Fusing point of the brine compared with clear water
It reduces, more heats can be absorbed, and cost is relatively low for other coolant liquids.
When producing ammonium fluoride, the first valve at anhydrous organic solvent tank liquid outlet is opened, is added into dry reaction kettle
Enter 400 kilograms of methanol, is then turned on the third valve of ammonia tank liquid outlet, 400 kilograms of liquefied ammonia is slowly added into reaction kettle
(speed 100L/min is added), temperature is controlled at 20 DEG C -30 DEG C.
The blender of reaction kettle bottom of chamber is opened, mixing speed is that 85 turns/min opens the coolant liquid after stirring 10min
The 8th valve being arranged at inlet, coolant liquid enters in the sandwich of reaction kettle cavity wall, is cooled down to reaction kettle, in kettle
Material temperature in whipping process gradually drops to 0 DEG C.When temperature is reduced to 0 DEG C, open at fluorination hydrogen gas tank gas outlet
The second valve, be stored in fluorination hydrogen gas tank in hydrogen fluoride be passed through in reaction kettle with the speed of 200L/min, ammonia and hydrogen fluoride
It is reacted in organic solvent, generates ammonium fluoride.Logical hydrogen fluoride gas stops logical fluorination hydrogen up to liquid pH=8 in kettle
Body.Due to will produce a large amount of heat in the generation of ammonium fluoride, a small amount of ammonia can be caused to disengage, received by condensing unit
Collection processing.
During logical hydrogen fluoride, there is a large amount of white solid ammonium fluoride to generate in kettle, reaction kettle cavity wall need to be used to lead to coolant liquid,
To the solvent in reaction kettle and kettle timely heat exchange is carried out to cool down, controlling reaction temperature at 10-30 DEG C, avoid in reaction kettle by
It is excessively violent in reacting, generate excessive pressure.
Stop after leading to hydrogen fluoride, the material in reaction kettle is centrifuged into (900 turns/min of centrifugal rotational speed), object with centrifuge
Material is separated by solid-liquid separation, and obtains the ammonium fluoride crude product of 970 kilograms or so of weight in wet base.Obtained mother liquor after separation of solid and liquid, by with mother liquor
Slot is collected, and mother liquor can be added in reaction kettle and recycle.
At 25 DEG C, the solubility of hydrofluoric acid in methyl alcohol is 50g, and the solubility of ammonia in methyl alcohol is 35g, the anhydrous fluorine
Change the solubility of ammonium in methyl alcohol and is less than 0.1g.
Obtained ammonium fluoride crude product is dried in vacuo, vacuum degree 0.08MPa, temperature 60 C, after drying 2 hours, is obtained
White solid fluorination ammonium product is 865 kilograms total, purity 99.4%, yield 99%.
Embodiment 2 is fluorinated the preparation of ammonium product
Difference lies in the organic solvent that embodiment 2 uses is ethyl alcohol to embodiment 2 with embodiment 1；The addition speed of liquefied ammonia
500L/min。
The solubility of 25 DEG C of hydrofluoric acid in ethanol is 50g, and the solubility of ammonia in ethanol is 35g, the anhydrous fluorination
The solubility of ammonium in ethanol is less than 0.1g.
It is 865 kilograms total to finally obtain white solid ammonium acid fluoride finished product, purity 99.4%, yield 99%.
Embodiment 3
Difference lies in use acetonitrile as organic solvent to embodiment 3 with embodiment 1 in embodiment 3；The addition of liquefied ammonia
Speed 10L/min.
Solubility of 25 DEG C of hydrofluoric acid in acetonitrile is 48g, and solubility of the ammonia in acetonitrile is 35g, the anhydrous fluorination
Solubility of the ammonium in acetonitrile is less than 0.1g.
Finally obtain white solid 866 kilograms of ammonium product of fluorination, purity 99.8%, yield 99%.
Embodiment 4
Embodiment 4 is distinguished as with embodiment 1：Embodiment 4 uses ethyl alcohol as organic solvent, the addition speed of liquefied ammonia
The Ventilation Rate of 300L/min, hydrofluoric acid gas are 500L/min, and duration of ventilation is 10 hours.Finally obtain white solid fluorination
Ammonium product is 865 kilograms total, purity 99.5%, yield 99%.
Embodiment 5
Embodiment 5 is distinguished as with embodiment 1：Embodiment 5 is using dichloromethane as organic solvent.
The solubility of 25 DEG C of hydrofluoric acid in methylene chloride is 48g, and the solubility of ammonia in methylene chloride is 35g, described
The solubility of anhydrous ammonium fluoride in methylene chloride is less than 0.1g.
Finally obtained white solid is fluorinated 861 kilograms of ammonium product, purity 99.3%, yield 99%.
Embodiment 6
Embodiment 6 is distinguished as with embodiment 1：The addition of liquefied ammonia is 50 kilograms in embodiment 6, and the addition of methanol is
950 kilograms, ammonia solution starts logical hydrofluoric acid gas in whipping process after temperature gradually drops to 10 DEG C, hydrofluoric acid gas
Ventilation Rate is 10L/min, leads to hydrofluoric acid until hydrofluoric acid is led in liquid pH=8, stopping in kettle.Finally obtained white solid fluorine
Change 86.6 kilograms of ammonium product, purity 99.3%, yield 99%.
Embodiment 7
Embodiment 7 is distinguished as with embodiment 6：In embodiment 71 is pressed using the warm and fine methanol of second:1 mass ratio mixing conduct
Organic solvent, ammonia solution start logical hydrofluoric acid gas in whipping process after temperature gradually drops to 5 DEG C, hydrofluoric acid gas
Ventilation Rate is 50L/min, leads to hydrofluoric acid gas until hydrofluoric acid is led in liquid pH=8, stopping in kettle.Finally obtained white is solid
Body is fluorinated ammonium product.
Embodiment 8
Embodiment 8 is distinguished as with embodiment 6：Embodiment 8 uses that dichloromethane, second is fine, methanol mixing, (mass ratio
1:1:1) organic solvent, ammonia solution is used as to start logical hydrofluoric acid gas after temperature gradually drops to 10 DEG C in whipping process,
The Ventilation Rate of hydrofluoric acid is 150L/min, leads to hydrofluoric acid until hydrofluoric acid gas is led in liquid pH=8, stopping in kettle.Final
The white solid fluorination ammonium product arrived.
It should be noted that herein, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that process, method, article or terminal device including a series of elements include not only those
Element, but also include other elements that are not explicitly listed, or further include for this process, method, article or end
The intrinsic element of end equipment.In the absence of more restrictions, being limited by sentence " including ... " or " including ... "
Element, it is not excluded that there is also other elements in process, method, article or the terminal device including the element.This
Outside, herein, " being more than ", " being less than ", " being more than " etc. are interpreted as not including this number；" more than ", " following ", " within " etc. understandings
It includes this number to be.
It should be noted that although the various embodiments described above have been described herein, it is not intended to limit
The scope of patent protection of the present invention.Therefore, based on the present invention innovative idea, to embodiment described herein carry out change and repair
Change, or using equivalent structure or equivalent flow shift made by description of the invention and accompanying drawing content, it directly or indirectly will be with
Upper technical solution is used in other related technical areas, is included within the scope of patent protection of the present invention.
Claims (10)
1. a kind of preparation method of ammonium fluoride, which is characterized in that be dissolved in ammonia and anhydrous hydrogen fluoride in organic solvent successively, nothing
Water hydrogen fluoride reacts the anhydrous ammonium fluoride of production with ammonia in the organic solvent；
The anhydrous hydrogen fluoride is higher than the anhydrous ammonium fluoride identical organic molten with solubility of the ammonia in the organic solvent
Solubility in agent.
2. preparation method according to claim 1, which is characterized in that the anhydrous hydrogen fluoride is with ammonia in the organic solvent
In solubility in 20g or more, solubility of the anhydrous ammonium fluoride in the organic solvent is in 1g or less.
3. preparation method according to claim 1 or 2, which is characterized in that the organic solvent includes methanol, ethyl alcohol, second
Or mixtures thereof nitrile, dichloromethane.
4. preparation method according to claim 1, which is characterized in that the preparation method comprises the following steps：
Ammonia solution is prepared：Liquefied ammonia is added in the organic solvent, is uniformly mixed, ammonia solution is configured；
Ammonium fluoride synthesizes：Hydrogen fluoride gas is passed through into ammonia solution, hydrogen fluoride is reacted with ammonia solution generates anhydrous ammonium fluoride, in vain
The anhydrous ammonium fluoride powder of color is precipitated from reaction solution.
5. preparation method according to claim 4, which is characterized in that in the ammonia solution preparation steps, the liquefied ammonia with
The mass ratio of the organic solvent is 5-50:50-95.
6. preparation method according to claim 4, which is characterized in that in the ammonium fluoride synthesis step, be passed through hydrogen fluoride
The pH value of gas to reaction solution terminates reaction after being 7-8.
7. preparation method according to claim 4, which is characterized in that in the ammonia solution preparation steps, the liquefied ammonia
Addition speed is 10L/min-500L/min；In the ammonium fluoride synthesis step, the draft speed of hydrogen fluoride is 10L/min-
500L/min。
8. preparation method according to claim 4, which is characterized in that in the ammonia solution preparation steps, feed temperature control
At 10 DEG C -30 DEG C, ammonia solution final temperature is controlled at 0 DEG C -10 DEG C system；In the ammonium fluoride synthesis step, reaction temperature control
At 10 DEG C -30 DEG C.
9. preparation method according to claim 4, which is characterized in that the preparation method further include solid-liquid separation step with
Vacuum drying step, the specific steps are：
It is separated by solid-liquid separation：The solution containing white anhydrous ammonium fluoride powder that ammonium fluoride synthesis step obtains be separated by solid-liquid separation
To ammonium fluoride crude product,
Vacuum drying：Ammonium fluoride crude product is subjected to reduced vacuum drying, obtains fluorination ammonium product.
10. a kind of system preparing ammonium fluoride by any the methods of claim 4-9, which is characterized in that including ammonia tank, fluorine
Change hydrogen gas tank, anhydrous organic solvent tank, reaction kettle, centrifuge, mother liquor tank, condensing unit, thermometer and pH meter；
The reaction kettle bottom of chamber is provided with blender, and liquefied ammonia inlet, hydrogen fluoride air inlet, nothing are offered above the reaction kettle
Aqueous organic solvent inlet, exhaust outlet, the first refluxing opening, the second refluxing opening, thermometer mouth and pH meter mouth, under the reaction kettle
Side offers reaction kettle liquid outlet, and the liquefied ammonia liquid outlet is connected by the first valve with the liquefied ammonia inlet opened up on reaction kettle
Logical, the fluorination hydrogen tank gas outlet is connected by the second valve with the fluorination hydrogen inlet opened up on reaction kettle, the nothing
Aqueous organic solvent tank liquid outlet is connected by third valve with the liquefied ammonia inlet opened up on reaction kettle, the reaction liquid from reactor
Mouth is connected by centrifuge and the 4th valve with the mother liquor tank inlet opened up on mother liquor tank, is opened up on the mother liquor tank
Mother liquor tank liquid outlet is connected by delivery pump with the first refluxing opening, and the thermometer is plugged in reaction kettle by thermometer mouth
In, the pH meter is plugged in a kettle by pH meter mouth；
The condensing unit includes condenser, gas-liquid separator and dump tank, and the exhaust outlet passes through condenser and the 5th
Valve is connected with the gas-liquid separator inlet that gas-liquid separator upper end opens up, and the gas-liquid separator lower end offers gas-liquid
The first liquid outlet of separator offers the second liquid outlet of gas-liquid separator, the dump tank upper end on the side of gas-liquid separator
Dump tank inlet is offered, the first liquid outlet of the gas-liquid separator is connected by the 6th valve with dump tank inlet,
The second liquid outlet of the gas-liquid separator is connected by the 7th valve with the second refluxing opening；
The reaction kettle cavity wall is sandwich, and coolant liquid inlet and coolant liquid are offered respectively in the reaction kettle cavity wall
Liquid outlet, coolant liquid inlet external refrigerant source are provided with the 8th valve at the coolant liquid inlet.
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| CN116859830A (en) * | 2023-03-27 | 2023-10-10 | 福建天甫电子材料有限公司 | Production management control system for electronic grade ammonium fluoride production |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1326552A1 (en) * | 1984-08-28 | 1987-07-30 | Днепропетровский химико-технологический институт им.Ф.Э.Дзержинского | Method of producing ammonium fluoride |
| CN102115095A (en) * | 2010-12-31 | 2011-07-06 | 应烈荣 | Production method of anhydrous ammonium hydrogen fluoride |
| CN103303941A (en) * | 2013-05-30 | 2013-09-18 | 福建省邵武市永飞化工有限公司 | Preparation method of ammonium fluoride |
| CN103539157A (en) * | 2013-10-31 | 2014-01-29 | 洛阳氟钾科技有限公司 | Process for recovering fluorine resource from decomposed potassium feldspar residue |
| CN105197959A (en) * | 2015-09-09 | 2015-12-30 | 洛阳国兴矿业科技有限公司 | Method of recovering fluorine resource in process of processing low-grade bauxite by chemical floatation method |
| CN105253907A (en) * | 2015-09-09 | 2016-01-20 | 洛阳国兴矿业科技有限公司 | Comprehensive utilization method for processing low-grade bauxite through chemical floating method |
-
2018
- 2018-08-20 CN CN201810948368.9A patent/CN108793192B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1326552A1 (en) * | 1984-08-28 | 1987-07-30 | Днепропетровский химико-технологический институт им.Ф.Э.Дзержинского | Method of producing ammonium fluoride |
| CN102115095A (en) * | 2010-12-31 | 2011-07-06 | 应烈荣 | Production method of anhydrous ammonium hydrogen fluoride |
| CN103303941A (en) * | 2013-05-30 | 2013-09-18 | 福建省邵武市永飞化工有限公司 | Preparation method of ammonium fluoride |
| CN103539157A (en) * | 2013-10-31 | 2014-01-29 | 洛阳氟钾科技有限公司 | Process for recovering fluorine resource from decomposed potassium feldspar residue |
| CN105197959A (en) * | 2015-09-09 | 2015-12-30 | 洛阳国兴矿业科技有限公司 | Method of recovering fluorine resource in process of processing low-grade bauxite by chemical floatation method |
| CN105253907A (en) * | 2015-09-09 | 2016-01-20 | 洛阳国兴矿业科技有限公司 | Comprehensive utilization method for processing low-grade bauxite through chemical floating method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116859830A (en) * | 2023-03-27 | 2023-10-10 | 福建天甫电子材料有限公司 | Production management control system for electronic grade ammonium fluoride production |
| CN116859830B (en) * | 2023-03-27 | 2024-01-26 | 福建天甫电子材料有限公司 | Production management control system for electronic grade ammonium fluoride production |
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| CN108793192B (en) | 2021-12-10 |
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