CN109353988A - The method that ammonium fluoride and the concentrated sulfuric acid are mixed with high concentration of hydrofluoric acid - Google Patents
The method that ammonium fluoride and the concentrated sulfuric acid are mixed with high concentration of hydrofluoric acid Download PDFInfo
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- CN109353988A CN109353988A CN201811340080.XA CN201811340080A CN109353988A CN 109353988 A CN109353988 A CN 109353988A CN 201811340080 A CN201811340080 A CN 201811340080A CN 109353988 A CN109353988 A CN 109353988A
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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
- C01B7/00—Halogens; Halogen acids
- C01B7/19—Fluorine; Hydrogen fluoride
- C01B7/191—Hydrogen fluoride
- C01B7/194—Preparation from ammonium fluoride
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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
- C01B7/00—Halogens; Halogen acids
- C01B7/19—Fluorine; Hydrogen fluoride
- C01B7/191—Hydrogen fluoride
- C01B7/195—Separation; Purification
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Abstract
The invention belongs to hydrofluoric acid preparation technical fields, especially ammonium fluoride and the concentrated sulfuric acid method that is mixed with high concentration of hydrofluoric acid, use ammonium fluoride and the concentrated sulfuric acid for raw material, three-level heating evaporation is carried out after mixing, every grade of evaporation selects different temperature and vacuum degree according to the characteristic of medium, it can effectively overcome the problems, such as that fluoroplastics liner is increased with temperature and resistance to negative pressure performance declines, the relatively low problem of single-stage evaporation efficiency is eliminated simultaneously, the hydrogen fluoride gas of evaporation obtains high concentration of hydrofluoric acid liquid through condensation, it can direct marketing or the raw materials for production as aluminum fluoride, remaining acid solution after the completion of evaporation is used for decomposing phosphate rock.
Description
Technical field
The invention belongs to hydrofluoric acid preparation technical field, especially ammonium fluorides and the concentrated sulfuric acid to be mixed with high concentration of hydrofluoric acid
Method.
Background technique
Wengfu technique is the direct One-step production anhydrous hydrofluoric acid of fluosilicic acid, uses the concentrated sulfuric acid and 45% concentration in the reactor
Silicate fluoride solution carry out heat resolve reaction, the product of decomposition reaction is gas SiF4With the nitration mixture with liquid HF and sulfuric acid
(or being fluosulfonic acid)；The nitration mixture of HF and sulfuric acid obtains anhydrous HF product through high temperature evaporation, purification；Leave the SiF4 gas of reactor
Body is absorbed with 18% fluosilicic acid material liquid of concentration to improve fluosilicic acid concentration and improve to being recycled after 45%, is then filtered
Reactor is sent to carry out decomposition reaction after falling the silica of precipitation.The nitration mixture of HF and sulfuric acid obtains concentration after distilling hydrogen fluoride
The fluorine-containing dilute sulfuric acid of 70%-75% is sent to phosphoric acid extraction slot for decomposing phosphate rock.This method technical process is simple, passes through control
The pyrolytical condition of the concentrated sulfuric acid and fluosilicic acid realizes the separation of ocratation and hydrogen fluoride in pyrogenic processes.The disadvantage is that fluosilicic acid point
The one way hydrogen fluoride theoretical yield of solution is only 33.3%, HF and H2O separative efficiency is also relatively low, therefore Matter Transfer treating capacity
Greatly, the loss of system fluorine is higher；In addition, hydrogen fluoride can also volatilize with ocratation during sulfuric acid decomposition fluosilicic acid, therefore right
The process regulation of decomposition is more demanding；In the process it is all high temperature strong corrosion medium, therefore device structure and material is wanted
Ask also higher, the high temperature evaporation equipment of especially HF, the excessively high service life that can shorten heater of temperature, temperature is low, can reduce
The yield of fluorine.
The ammonia process two-step process of phosphorus is opened to contain fluorine gas containing what is be discharged in the solution of ammonia, ammonium fluoride absorption phophatic fertilizer production process
Body is contained (NH4)2SiF6The ammonium fluosilicate slurry of crystal, is obtained by filtration ammonium fluosilicate solid；Or with H2SiF66%~
26% fluosilicic acid is raw material, is passed through gas ammonia progress neutralization reaction and obtains (NH4)2SiF6Solution is concentrated by evaporation to precipitation by solution
(NH4)2SiF6Ammonium fluosilicate solid is obtained by filtration in enriching slurry by crystal.Saturation fluorine is added in ammonium fluosilicate solid and liquefied ammonia simultaneously
Change ammonium salt solution progress ammonolysis reaction to obtain containing NH4F crystal and SiO2·nH2The ammonium fluoride slurry of O solid, to the NH of the slurry4F
Crystal and SiO2·nH2O solid, which carries out physical separation and filtering, can respectively obtain NH4F crystal and SiO2·nH2O silicon slag；NH4F
Crystal carries out reacting dissolution with sulfuric acid, then evaporates HF by circulating-heating, generates thick hydrogen fluoride gas, then washed net
Change, condensation obtains anhydrous hydrogen fluoride.The main component of acidolysis raffinate is the mixture of sulfuric acid and ammonium hydrogen sulfate, which adds
Enter phosphoric acid extraction slot to be recycled.This method is the disadvantage is that circulating-heating flow is big, and internal circulating load is larger, when equipment leaks
Security risk is big；Microwave heating is taken, mixed acid solution thermal transition low efficiency, the medium heat-transfer performance in device are poor, heating speed
Rate is slow, and hydrofluoric acid resolution factor is low, while nitration mixture flow behavior will lead to the heat that microwave generates and can not take away in time, concentrate on adding
Hot arc is presented at mouth, and local temperature raising is caused to burn out fluoroplastics lining.
Summary of the invention
In order to solve the above technical problems existing in the prior art, the present invention provides ammonium fluoride and the concentrated sulfuric acid is mixed with
The method of high concentration of hydrofluoric acid, comprising the following steps:
The method that ammonium fluoride and the concentrated sulfuric acid are mixed with high concentration of hydrofluoric acid, comprising the following steps:
(1) it mixes: ammonium fluoride crystal and the concentrated sulfuric acid is added to dissolving tank, carried out under the conditions of adding water to be placed in 60-120 DEG C anti-
It answers, obtains mixed solution；
(2) level-one is evaporated: mixed solution feeding level-one evaporator being reacted, temperature is 120-140 DEG C, and vacuum degree is
60-80KPa obtains level-one evaporation liquid and hydrogen fluoride gas A；
(3) dual evaporation: level-one evaporation liquid is sent into secondary evaporimeter and is reacted, temperature is 150-170 DEG C, vacuum degree
For 45-60KPa, dual evaporation liquid and hydrogen fluoride gas B are obtained；
(4) three-level is evaporated: dual evaporation liquid feeding three-level evaporator being reacted, temperature is 170-190 DEG C, vacuum degree
≤ 45KPa obtains three-level evaporation liquid and hydrogen fluoride gas C；
(5) it condenses: hydrogen fluoride gas A, hydrogen fluoride gas B, hydrogen fluoride gas C being respectively fed to condenser condensation, obtain liquid
The thick hydrofluoric acid of body obtains anhydrous hydrogen fluoride after refining.
The ammonium fluoride crystal additional amount is 5t/h, and concentrated sulfuric acid additional amount is 14.57-15.89t/h, and the additional amount of water is
0.1-0.5t/h。
The level-one evaporator, secondary evaporimeter and three-level evaporator are tube heater.
210 DEG C, maximum pressure 1.5MPa of the tube heater maximum temperature, 190 DEG C of medium maximum temperature, medium is taken
The mode that overflow goes out.
The three-level evaporation liquid is sent into residual sour geosyncline, prepares phosphoric acid by wet process for decomposing phosphate rock.
The hydrogen fluoride gas A that the level-one evaporator obtains is sent into condenser by vacuum pump 1.
The hydrogen fluoride gas B that the secondary evaporimeter obtains is sent into condenser by vacuum pump 2.
The hydrogen fluoride gas C that the three-level evaporator obtains is sent into condenser by vacuum pump 3.
Beneficial effect
1. using the three-level evaporation of different temperatures, different vacuum degrees, every grade of evaporator size is substantially reduced, can be effectively improved
The ability of equipment high temperature resistant and negative pressure deformation.
2. the evaporation rate for hydrogen fluoride in mixed acid solution is influenced by hydrogen fluoride content variation in medium, adjust in due course
Evaporation efficiency and hydrogen fluoride yield greatly improved in evaporating temperature and vacuum degree.
3. the present invention uses ammonium fluoride and the concentrated sulfuric acid for raw material, three-level heating evaporation, every grade of evaporation basis are carried out after mixing
The characteristic of medium selects different temperature and vacuum degree, can effectively overcome fluoroplastics liner with temperature raising and under resistance to negative pressure performance
The problem of drop, while the relatively low problem of single-stage evaporation efficiency is eliminated, the hydrogen fluoride gas of evaporation obtains high concentration of hydrogen through condensation
Fluoric acid liquid, can direct marketing or the raw materials for production as aluminum fluoride, remaining acid solution after the completion of evaporating is used for decomposing phosphate rock.
It is 120-140 DEG C by adjusting temperature 4. the present invention heats mixed solution using level-one evaporator, vacuum
After degree is 60-80KPa, so that the ammonium fluoride crystal in nitration mixture can be completely dissolved, hydrogen fluoride and water can be escaped, the evolution of hydrogen fluoride
Rate is 70-80%；After level-one evaporation liquid enters dual evaporation heating, the hydrogen fluoride in solution and water content are reduced at this time, are passed through
Temperature is adjusted to 150-170 DEG C, it is effective to improve the evaporation rate for protecting hydrogen fluoride and evaporation speed after vacuum degree is 45-60KPa
Degree, the evolution rate of hydrogen fluoride reaches 80-90%, and after dual evaporation liquid enters three-level evaporator, adjustment temperature is 170-190 DEG C,
After vacuum degree≤45KPa, so that the evolution rate of final hydrogen fluoride reaches 90% or more.
Detailed description of the invention
Fig. 1 is the process flow chart that ammonium fluoride of the present invention and the concentrated sulfuric acid are mixed with high concentration of hydrofluoric acid.
Specific embodiment
Tuberculosis specific embodiment is limited technical solution of the present invention is further below, but claimed
Range is not only limited to made description.
Embodiment 1
The method that ammonium fluoride and the concentrated sulfuric acid are mixed with high concentration of hydrofluoric acid, comprising the following steps:
(1) it mixes: ammonium fluoride crystal and the concentrated sulfuric acid being added to dissolving tank, reacted under the conditions of adding water to be placed in 60 DEG C,
Obtain mixed solution；
(2) level-one is evaporated: mixed solution feeding level-one evaporator being reacted, temperature is 120 DEG C, and vacuum degree is
60KPa obtains level-one evaporation liquid and hydrogen fluoride gas A；
(3) dual evaporation: level-one evaporation liquid is sent into secondary evaporimeter and is reacted, temperature is 150 DEG C, and vacuum degree is
45KPa obtains dual evaporation liquid and hydrogen fluoride gas B；
(4) three-level is evaporated: dual evaporation liquid feeding three-level evaporator being reacted, temperature is 170 DEG C, and vacuum degree is
10KPa obtains three-level evaporation liquid and hydrogen fluoride gas C；
(5) it condenses: hydrogen fluoride gas A, hydrogen fluoride gas B, hydrogen fluoride gas C being respectively fed to condenser condensation, obtain liquid
The thick hydrofluoric acid of body obtains anhydrous hydrogen fluoride after refining.
The ammonium fluoride crystal additional amount is 5t/h, and concentrated sulfuric acid additional amount is 14.57t/h, and the additional amount of water is 0.1t/h.
The level-one evaporator, secondary evaporimeter and three-level evaporator are tube heater.
Embodiment 2
The method that ammonium fluoride and the concentrated sulfuric acid are mixed with high concentration of hydrofluoric acid, comprising the following steps:
(1) it mixes: ammonium fluoride crystal and the concentrated sulfuric acid being added to dissolving tank, reacted under the conditions of adding water to be placed in 120 DEG C,
Obtain mixed solution；
(2) level-one is evaporated: mixed solution feeding level-one evaporator being reacted, temperature is 140 DEG C, and vacuum degree is
80KPa obtains level-one evaporation liquid and hydrogen fluoride gas A；
(3) dual evaporation: level-one evaporation liquid is sent into secondary evaporimeter and is reacted, temperature is 170 DEG C, and vacuum degree is
60KPa obtains dual evaporation liquid and hydrogen fluoride gas B；
(4) three-level is evaporated: dual evaporation liquid feeding three-level evaporator being reacted, temperature is 190 DEG C, and vacuum degree is
45KPa obtains three-level evaporation liquid and hydrogen fluoride gas C；
(5) it condenses: hydrogen fluoride gas A, hydrogen fluoride gas B, hydrogen fluoride gas C being respectively fed to condenser condensation, obtain liquid
The thick hydrofluoric acid of body obtains anhydrous hydrogen fluoride after refining.
The ammonium fluoride crystal additional amount is 5t/h, and concentrated sulfuric acid additional amount is 15.89t/h, and the additional amount of water is 0.5t/h.
The level-one evaporator, secondary evaporimeter and three-level evaporator are tube heater.
Embodiment 3
The method that ammonium fluoride and the concentrated sulfuric acid are mixed with high concentration of hydrofluoric acid, comprising the following steps:
(1) it mixes: ammonium fluoride crystal and the concentrated sulfuric acid being added to dissolving tank, reacted under the conditions of adding water to be placed in 80 DEG C,
Obtain mixed solution；
(2) level-one is evaporated: mixed solution feeding level-one evaporator being reacted, temperature is 130 DEG C, and vacuum degree is
70KPa obtains level-one evaporation liquid and hydrogen fluoride gas A；
(3) dual evaporation: level-one evaporation liquid is sent into secondary evaporimeter and is reacted, temperature is 160 DEG C, and vacuum degree is
55KPa obtains dual evaporation liquid and hydrogen fluoride gas B；
(4) three-level is evaporated: dual evaporation liquid feeding three-level evaporator being reacted, temperature is 180 DEG C, and vacuum degree is
35KPa obtains three-level evaporation liquid and hydrogen fluoride gas C；
(5) it condenses: hydrogen fluoride gas A, hydrogen fluoride gas B, hydrogen fluoride gas C being respectively fed to condenser condensation, obtain liquid
The thick hydrofluoric acid of body obtains anhydrous hydrogen fluoride after refining.
The ammonium fluoride crystal additional amount is 5t/h, and concentrated sulfuric acid additional amount is 14.85/h, and the additional amount of water is 0.25t/h.
The level-one evaporator, secondary evaporimeter and three-level evaporator are tube heater.
The three-level evaporation liquid is sent into residual sour geosyncline, prepares phosphoric acid by wet process for decomposing phosphate rock.
Test example 1
Ammonium fluoride amount 5t/h, concentrated sulfuric acid 14.57t/h, add water 0.25t/h, and mixed solution temperature is about 95 DEG C after reaction, object
Material is delivered to level-one evaporator, controls 130 DEG C of temperature, vacuum degree 70KPa, and the evolution rate of level-one evaporator hydrogen fluoride is at this time
76.5%；160 DEG C of secondary evaporimeter temperature, vacuum degree 50KPa, the evolution rate 88.4% of hydrogen fluoride after dual evaporation；Three-level
Evaporator, 180 DEG C of temperature, vacuum degree 37KPa, final hydrogen fluoride evolution rate is 93.7%, and residual acid fluorinated volume is 1.08%, cold
Hydrofluoric acid concentration 94.4% after solidifying.
Test example 2
Ammonium fluoride amount 5t/h, concentrated sulfuric acid 17.22t/h, add water 0.5t/h, and mixed solution temperature is about 117 DEG C after reaction, object
Material is delivered to level-one evaporator, controls 120 DEG C of temperature, vacuum degree 60KPa, and the evolution rate of level-one evaporator hydrogen fluoride is at this time
73.9%；150 DEG C of secondary evaporimeter temperature, vacuum degree 45KPa, the evolution rate 89.3% of hydrogen fluoride after dual evaporation；Three-level
Evaporator, 190 DEG C of temperature, vacuum degree 35KPa, final hydrogen fluoride evolution rate is 94.2%, and residual acid fluorinated volume is 1.00%, cold
Hydrofluoric acid concentration 91.7% after solidifying.
Test example 3
Water 0.1t/h is added in ammonium fluoride amount 5t/h, concentrated sulfuric acid 15.89t/h, and mixed solution temperature is about 72 DEG C after reaction,
Material is delivered to level-one evaporator, controls 140 DEG C of temperature, vacuum degree 80KPa, and the evolution rate of level-one evaporator hydrogen fluoride is at this time
75.1%；170 DEG C of secondary evaporimeter temperature, vacuum degree 55KPa, the evolution rate 90.3% of hydrogen fluoride after dual evaporation；Three-level
Evaporator, 190 DEG C of temperature, vacuum degree 30KPa, final hydrogen fluoride evolution rate is 92.1%, and residual acid fluorinated volume is 1.34%, cold
Hydrofluoric acid concentration 97.2% after solidifying.
It is important to point out that, above embodiments and test example are only limitted to do further technical solution of the present invention herein
Elaboration and understanding, should not be understood as it is further to technical solution of the present invention limited, what those skilled in the art made
The innovation and creation of non-protruding essential characteristics and marked improvement still fall within protection category of the invention.
Claims (5)
1. the method that ammonium fluoride and the concentrated sulfuric acid are mixed with high concentration of hydrofluoric acid, which comprises the following steps:
(1) it mixes: ammonium fluoride crystal and the concentrated sulfuric acid being added to dissolving tank, reacted under the conditions of adding water to be placed in 60-120 DEG C,
Obtain mixed solution；
(2) level-one is evaporated: mixed solution feeding level-one evaporator being reacted, temperature is 120-140 DEG C, vacuum degree 60-
80KPa obtains level-one evaporation liquid and hydrogen fluoride gas A；
(3) dual evaporation: level-one evaporation liquid is sent into secondary evaporimeter and is reacted, temperature is 150-170 DEG C, and vacuum degree is
45-60KPa obtains dual evaporation liquid and hydrogen fluoride gas B；
(4) three-level is evaporated: dual evaporation liquid feeding three-level evaporator to be reacted, temperature is 170-190 DEG C, vacuum degree≤
45KPa obtains three-level evaporation liquid and hydrogen fluoride gas C；
(5) it condenses: hydrogen fluoride gas A, hydrogen fluoride gas B, hydrogen fluoride gas C being respectively fed to condenser condensation, obtain liquid crude
Hydrofluoric acid obtains anhydrous hydrogen fluoride after refining.
2. the method that ammonium fluoride as described in claim 1 and the concentrated sulfuric acid are mixed with high concentration of hydrofluoric acid, which is characterized in that described
Ammonium fluoride crystal additional amount is 5t/h, and concentrated sulfuric acid additional amount is 14.57-15.89t/h, and the additional amount of water is 0.1-0.5t/h.
3. the method that ammonium fluoride as described in claim 1 and the concentrated sulfuric acid are mixed with high concentration of hydrofluoric acid, which is characterized in that described
Level-one evaporator, secondary evaporimeter and three-level evaporator are tube heater.
4. the method that ammonium fluoride as claimed in claim 3 and the concentrated sulfuric acid are mixed with high concentration of hydrofluoric acid, which is characterized in that described
210 DEG C of tube heater maximum temperature, maximum pressure 1.5MPa, 190 DEG C of medium maximum temperature, the side that medium takes overflow to go out
Formula.
5. the method that ammonium fluoride as described in claim 1 and the concentrated sulfuric acid are mixed with high concentration of hydrofluoric acid, which is characterized in that described
Three-level evaporates the residual sour geosyncline of liquid feeding, prepares phosphoric acid by wet process for decomposing phosphate rock.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112456442A (en) * | 2020-12-11 | 2021-03-09 | 昆山市诚鑫化工有限公司 | Preparation method of saturated hydrofluoric acid |
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| CN106185817A (en) * | 2016-07-12 | 2016-12-07 | 中南大学 | A kind of method reclaiming Fluohydric acid. from fluorine-containing silicic acid waste water |
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