CN109795991B - Safe and energy-saving purification treatment process for fluorosulfuric acid - Google Patents
Safe and energy-saving purification treatment process for fluorosulfuric acid Download PDFInfo
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- CN109795991B CN109795991B CN201910287526.5A CN201910287526A CN109795991B CN 109795991 B CN109795991 B CN 109795991B CN 201910287526 A CN201910287526 A CN 201910287526A CN 109795991 B CN109795991 B CN 109795991B
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- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000000746 purification Methods 0.000 title claims abstract description 18
- UQSQSQZYBQSBJZ-UHFFFAOYSA-N fluorosulfonic acid Chemical compound OS(F)(=O)=O UQSQSQZYBQSBJZ-UHFFFAOYSA-N 0.000 title claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 272
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 86
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims abstract description 50
- 238000001704 evaporation Methods 0.000 claims abstract description 38
- 230000008020 evaporation Effects 0.000 claims abstract description 38
- 239000002253 acid Substances 0.000 claims abstract description 34
- 239000007789 gas Substances 0.000 claims abstract description 32
- 238000010521 absorption reaction Methods 0.000 claims abstract description 27
- 238000002156 mixing Methods 0.000 claims abstract description 24
- 238000009833 condensation Methods 0.000 claims abstract description 18
- 230000005494 condensation Effects 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 18
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 11
- 239000011737 fluorine Substances 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 9
- 238000006115 defluorination reaction Methods 0.000 claims abstract description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 10
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 9
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 9
- 239000010959 steel Substances 0.000 claims description 8
- 229910000831 Steel Inorganic materials 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- 229910000976 Electrical steel Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims 1
- OBTWBSRJZRCYQV-UHFFFAOYSA-N sulfuryl difluoride Chemical compound FS(F)(=O)=O OBTWBSRJZRCYQV-UHFFFAOYSA-N 0.000 claims 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 abstract 1
- 230000008901 benefit Effects 0.000 description 5
- 239000000872 buffer Substances 0.000 description 5
- 238000004821 distillation Methods 0.000 description 5
- 235000011149 sulphuric acid Nutrition 0.000 description 5
- 239000001117 sulphuric acid Substances 0.000 description 5
- 239000012141 concentrate Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 238000003795 desorption Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000010924 continuous production Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000011549 displacement method Methods 0.000 description 1
- 210000001035 gastrointestinal tract Anatomy 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000004400 mucous membrane Anatomy 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 210000003491 skin Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses a safe and energy-saving purification treatment process of sulfuric acid containing fluorine, which comprises a preheating evaporation section, a mixing removal section and a sulfuric acid concentration section; the preheating evaporation section evaporates the raw material acid under vacuum condition to increase the concentration of sulfuric acid, the concentrated sulfuric acid is sent to the mixing removal section, and hydrogen fluoride steam generated in the evaporation process enters a hydrogen fluoride absorption tower; the mixed removal section sends the sulfuric acid from the preheating evaporation section and the sulfuric acid from the sulfuric acid concentration section to a removal rectifying tower, hydrogen fluoride contained in the sulfuric acid is removed in a mixed manner, the sulfuric acid after defluorination is sent to the sulfuric acid concentration section, and hydrogen fluoride steam generated in the removal process enters a hydrogen fluoride absorption tower; and the sulfuric acid concentration section sends concentrated sulfuric acid from the mixing and removing section to a sulfuric acid concentrator, the concentration of the sulfuric acid is increased under a high vacuum condition, one part of the obtained high-concentration sulfuric acid is continuously extracted out of the system, the other part of the obtained high-concentration sulfuric acid is sent back to the mixing and removing section to be mixed, and tail gas enters a tail gas condensation tower and a gas washing tower and is discharged after reaching the standard.
Description
Technical Field
The invention relates to the field of chemical post-treatment, in particular to a safe and energy-saving purification treatment process of sulfuric acid containing fluorine.
Background
Hydrogen fluoride, a colorless gas with pungent odor, has toxicity and strong corrosivity in itself and its aqueous solution, can be absorbed through skin, mucous membrane, respiratory tract and gastrointestinal tract, and can produce strong irritation and corrosion to these parts, which can cause burn. The existing hydrogen fluoride recovery process mostly adopts a concentrated sulfuric acid displacement method, so that a large amount of fluorine-containing waste sulfuric acid liquid is generated, the treatment is extremely difficult, huge environment-friendly treatment cost can be brought to enterprises, and the environment can be greatly polluted.
In view of the above situation, the invention provides a safe and energy-saving process for purifying sulfuric acid containing fluorine, which can separate hydrofluoric acid and sulfuric acid as impurities, simultaneously concentrate dilute sulfuric acid into concentrated sulfuric acid, absorb steam generated in the concentration process through an absorption system, reduce tail gas emission, improve recovery efficiency, has the advantages of simple method, continuous production, good separation and concentration effects, improved operating environment, saved operating cost, safe, stable, energy-saving, environment-friendly and no secondary pollution when the system operates under negative pressure.
Disclosure of Invention
In order to solve the technical problem, the invention provides a safe and energy-saving purification treatment process of sulfuric acid containing fluorine, which comprises a preheating evaporation section, a mixing removal section and a sulfuric acid concentration section;
the preheating evaporation section evaporates the raw material acid under vacuum condition to increase the concentration of sulfuric acid, the concentrated sulfuric acid is sent to the mixing removal section, and hydrogen fluoride steam generated in the evaporation process enters a hydrogen fluoride absorption tower;
the mixed removal section sends the sulfuric acid from the preheating evaporation section and the sulfuric acid from the sulfuric acid concentration section to a removal rectifying tower, hydrogen fluoride contained in the sulfuric acid is removed in a mixed manner, the sulfuric acid after defluorination is sent to the sulfuric acid concentration section, and hydrogen fluoride steam generated in the removal process enters a hydrogen fluoride absorption tower;
and the sulfuric acid concentration section sends concentrated sulfuric acid from the mixing and removing section to a sulfuric acid concentrator, the concentration of the sulfuric acid is increased under a high vacuum condition, one part of the obtained high-concentration sulfuric acid is continuously extracted out of the system, the other part of the obtained high-concentration sulfuric acid is sent back to the mixing and removing section to be mixed, and tail gas enters a tail gas condensation tower and a gas washing tower and is discharged after reaching the standard.
As a preferred technical scheme, the preheating evaporation section comprises a preheater and a preheating evaporator.
As a preferable technical scheme, the preheater is made of silicon carbide, and the pre-evaporation evaporator is made of silicon carbide or steel sintered PTFE.
As a preferable technical scheme, the sulfuric acid concentration of the raw material acid is 30-40 wt%, and the hydrogen fluoride concentration is 10-20 wt%.
As a preferable technical scheme, the concentration of the raw material acid is increased to 80-88 wt% in the preheating evaporation section.
As a preferable technical solution, the hydrogen fluoride absorption tower converts hydrogen fluoride into hydrofluoric acid by condensation absorption.
As a preferable technical scheme, the sulfuric acid concentration of the sulfuric acid concentration section is increased to 90-95 wt%.
As a preferable technical scheme, the concentration of the sulfuric acid in the mixed removal section is 88-90 wt%.
As a preferable technical scheme, the material of the desorption and rectification tower is steel sintered PTFE.
In a preferred embodiment, the sulfuric acid concentrator is made of silicon carbide.
Has the advantages that: the invention provides a safe and energy-saving purification treatment process of sulfuric acid containing fluorine, which can separate hydrofluoric acid and sulfuric acid as impurities, simultaneously concentrate dilute sulfuric acid into concentrated sulfuric acid, absorb steam generated in the concentration process through an absorption system, reduce tail gas emission, improve recovery efficiency, has the advantages of simple method, continuous production, good separation and concentration effects, improved operation environment, saved operation cost, safe, stable, energy-saving and environment-friendly operation of the system under negative pressure, and no secondary pollution.
Drawings
To further illustrate the safe and energy-efficient fluorosulfuric acid purification process flow provided in the present invention, the accompanying drawings are provided, it being noted that the drawings provided in the present invention are only selected from individual examples of all drawings, and are not intended to limit the claims, and all other corresponding figures obtained from the drawings provided in the present application should be considered as falling within the protection scope of the present application
FIG. 1 is a flow chart of the process for the purification treatment of fluorosulfuric acid.
Detailed Description
The present invention will be further understood in conjunction with the following detailed description of preferred embodiments of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. To the extent that a definition of a particular term disclosed in the prior art is inconsistent with any definitions provided herein, the definition of the term provided herein controls.
As used herein, a feature that does not define a singular or plural form is also intended to include a plural form of the feature unless the context clearly indicates otherwise. It will be further understood that the term "comprising," as used herein, is synonymous with "including," "comprising," "having," "including," and/or "containing," and the like, when used in this specification, means that the recited composition, step, method, article, or apparatus, but does not preclude the presence or addition of one or more other compositions, steps, methods, articles, or apparatuses. Furthermore, the use of "preferred," "preferably," "more preferred," etc., when describing embodiments of the present application, is meant to refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. In addition, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
The meaning of "and/or" in the present invention means that the respective single or both of them exist individually or in combination.
The meaning of "inside and outside" in the present invention means that the direction pointing to the inside of the device is inside and vice versa with respect to the device itself, and is not a specific limitation of the mechanism of the apparatus of the present invention.
The meaning of "left and right" in the present invention means that when the reader is facing the drawings, the left side of the reader is left, and the right side of the reader is right, and is not a specific limitation on the mechanism of the apparatus of the present invention.
The term "connected" as used herein may mean either a direct connection between the components or an indirect connection between the components via other components.
The invention provides a safe and energy-saving purification treatment process of sulfuric acid containing fluorine, which comprises a preheating evaporation section, a mixing removal section and a sulfuric acid concentration section;
the preheating evaporation section evaporates the raw material acid under vacuum condition to increase the concentration of sulfuric acid, the concentrated sulfuric acid is sent to the mixing removal section, and hydrogen fluoride steam generated in the evaporation process enters a hydrogen fluoride absorption tower;
the mixed removal section sends the sulfuric acid from the preheating evaporation section and the sulfuric acid from the sulfuric acid concentration section to a removal rectifying tower, hydrogen fluoride contained in the sulfuric acid is removed in a mixed manner, the sulfuric acid after defluorination is sent to the sulfuric acid concentration section, and hydrogen fluoride steam generated in the removal process enters a hydrogen fluoride absorption tower;
and the sulfuric acid concentration section sends concentrated sulfuric acid from the mixing and removing section to a sulfuric acid concentrator, the concentration of the sulfuric acid is increased under a high vacuum condition, one part of the obtained high-concentration sulfuric acid is continuously extracted out of the system, the other part of the obtained high-concentration sulfuric acid is sent back to the mixing and removing section to be mixed, and tail gas enters a tail gas condensation tower and a gas washing tower and is discharged after reaching the standard.
The process for purifying a fluorosulfuric acid of the present invention will be described in detail with reference to FIG. 1.
Preheating evaporation section
The main equipment in the preheating evaporation section in the application comprises a preheater and a preheating evaporator, and raw material acid is continuously conveyed to the preheater from a storage tank through a high-level metering tank through a feed pump for preheating.
In some preferred embodiments, the raw acid is fed at 850 kg/hr, the sulfuric acid concentration is 30 to 40 wt%, and the hydrogen fluoride concentration is 10 to 20 wt%.
In some preferred embodiments, the preheater is made of silicon carbide, the operating pressure is normal pressure, the shell-side temperature is 90-95 ℃, and the tube-side temperature is 25-60 ℃.
The preheated raw material acid enters a pre-evaporation evaporator, most of water is removed under the vacuum condition, the sulfuric acid with the increased concentration automatically flows into a mixed removal section, hydrogen fluoride steam generated in the evaporation process enters a hydrogen fluoride absorption tower, and hydrofluoric acid obtained after condensation and absorption is collected to a hydrofluoric acid cache tank for further treatment.
In some preferred embodiments, the material of the pre-evaporation evaporator is silicon carbide or steel sintered tetrafluoro, the operating pressure is 0.012MPa, and the operating temperature is 140-160 ℃.
In some preferred embodiments, the preheating evaporation section raises the concentration of the raw material acid to 80-88 wt%; further preferably, the concentration of the raw material acid is increased to 86-88 wt% by the preheating evaporation section.
In some preferred embodiments, the hydrogen fluoride absorber column concentrates hydrogen fluoride by condensation; further preferably, the hydrogen fluoride-absorbing column concentrates hydrogen fluoride by multiple condensation.
In some preferred embodiments, the hydrogen fluoride absorption tower is made of steel lined tetrafluoro, the operation pressure is normal pressure, and the operation temperature is not higher than 40 ℃.
Hybrid removal section
Mix the capital equipment of desorption section in this application for desorption rectifying column, the sulphuric acid that comes from preheating evaporation zone and sulphuric acid concentration section mixes here, sulphuric acid and hydrogen fluoride intensive separation under the high temperature high enriched condition, sulphuric acid flow in sulphuric acid concentration section after the separation, hydrogen fluoride steam gets into the hydrogen fluoride absorption tower, and the hydrofluoric acid that obtains after the condensation absorption is collected to hydrofluoric acid buffer tank, stays to wait for further processing.
In some preferred embodiments, the sulfuric acid concentration of the mixed removal stage is from 88 to 90 wt%.
In some preferred embodiments, the material of the dephlegmation and rectification tower is steel sintered tetrafluoro, the operation pressure is normal pressure, and the operation temperature is not higher than 150 ℃.
Sulfuric acid concentration section
The main equipment of the sulfuric acid concentration section in the application comprises a sulfuric acid concentrator, a concentrated acid cooler, a tail gas condensation tower and a gas washing tower. After the sulfuric acid from the stripping distillation tower is concentrated under the condition of high vacuum, one part of the sulfuric acid is continuously extracted and enters a concentrated acid cooler, the cooled concentrated sulfuric acid is transferred into a finished acid tank by a finished acid pump, and the other part of the sulfuric acid is returned to the mixing stripping section to improve the concentration of the sulfuric acid in the mixed stripping section. And tail gas generated in the concentration process enters a tail gas condensing tower, and residual gas after condensation enters a gas washing tower and is discharged after the treatment reaches the standard.
In some preferred embodiments, the sulfuric acid concentration stage raises the sulfuric acid concentration to 90-95 wt%; further preferably, the sulfuric acid concentration section raises the sulfuric acid concentration to 91-94 wt%.
In some preferred embodiments, the sulfuric acid concentrator, the concentrated acid cooler and the tail gas condensing tower are made of silicon carbide, and the gas washing tower is made of steel sintered tetrafluoro.
In some preferred embodiments, the operating pressure of the sulfuric acid concentrator is 0.008MPa, and the operating temperature is 170-190 ℃.
In some preferred embodiments, the concentrated acid cooler has an operating pressure of 0.008MPa, a shell side temperature of 25 to 35 ℃, and a tube side temperature of 50 to 180 ℃.
In some preselected embodiments, the tail gas condenser is operated at a pressure of 0.008MPa and at a temperature of no more than 120 ℃.
Examples
The technical solution of the present invention is described in detail by the following examples, but the scope of the present invention is not limited to the examples.
Example 1
Embodiment 1 provides a safe and energy-saving purification treatment process of fluorosulfuric acid, which comprises the following steps:
a. preheating an evaporation section: the raw material acid is continuously sent to a preheater for preheating through a storage tank and a high-level metering tank by a feed pump, wherein the shell side temperature of the preheater is 90 ℃, and the tube side temperature is 40 ℃. The sulfuric acid content of the raw material acid was 35 wt%, the hydrogen fluoride content was 16 wt%, and the feed amount was 850 kg/h, i.e., 20 tons/day. The preheated raw material acid enters a pre-evaporation evaporator, most of water is removed under the operating conditions of pressure of 0.012MPa and temperature of 150 ℃, the concentration of sulfuric acid is increased to 85 wt% and then automatically flows into a mixing removal section, hydrogen fluoride steam generated in the evaporation process enters a hydrogen fluoride absorption tower, and hydrofluoric acid obtained after condensation and absorption is collected to a hydrofluoric acid buffer tank for further treatment.
b. A mixing and removing section: mixing sulfuric acid from the preheating evaporation section and the sulfuric acid concentration section in a removal distillation tower to obtain sulfuric acid with the concentration of 88 wt%, fully separating the sulfuric acid from hydrogen fluoride under the conditions of high temperature and high concentration, enabling the separated sulfuric acid to flow into the sulfuric acid concentration section, enabling hydrogen fluoride steam to enter a hydrogen fluoride absorption tower, collecting hydrofluoric acid obtained after condensation and absorption to a hydrofluoric acid buffer tank, and reserving for further treatment.
c. A sulfuric acid concentration section: the sulfuric acid from the removal distillation tower is sent to a sulfuric acid concentrator, after the sulfuric acid is concentrated to 93 wt% under the operating conditions of the pressure of 0.008MPa and the temperature of 180 ℃, one part of the sulfuric acid is continuously extracted and sent to a concentrated acid cooler, the operating pressure of the concentrated acid cooler is 0.008MPa, the shell side temperature is 25 ℃, the tube side temperature is 100 ℃, the cooled concentrated sulfuric acid is transferred to a finished product acid tank by a finished product acid pump, and the other part of the sulfuric acid is returned to a mixing removal section to improve the concentration of the sulfuric acid in the concentrated sulfuric acid. And tail gas generated in the concentration process enters a tail gas condensing tower, and residual gas after condensation enters a gas washing tower and is discharged after the treatment reaches the standard.
After treatment according to this example, about 310 kg of 93 wt% concentrated sulfuric acid and 133 kg of 25 wt% hydrofluoric acid per hour can be produced.
Example 2
Embodiment 2 provides a safe and energy-saving purification treatment process of fluorosulfuric acid, which comprises the following steps:
a. preheating an evaporation section: the raw material acid is continuously sent to a preheater for preheating through a storage tank and a high-level metering tank by a feed pump, wherein the shell side temperature of the preheater is 95 ℃, and the tube side temperature is 50 ℃. The sulfuric acid content of the raw material acid was 35 wt%, the hydrogen fluoride content was 16 wt%, and the feed amount was 850 kg/h, i.e., 20 tons/day. The preheated raw material acid enters a pre-evaporation evaporator, most of water is removed under the operating conditions of pressure of 0.012MPa and temperature of 160 ℃, the concentration of sulfuric acid is increased to 86 wt% and then automatically flows into a mixing removal section, hydrogen fluoride steam generated in the evaporation process enters a hydrogen fluoride absorption tower, and hydrofluoric acid obtained after condensation and absorption is collected to a hydrofluoric acid buffer tank for further treatment.
b. A mixing and removing section: sulfuric acid from the preheating evaporation section and the sulfuric acid concentration section is mixed in a removal distillation tower to obtain sulfuric acid with the concentration of 89 wt%, the sulfuric acid and hydrogen fluoride are fully separated under the condition of high temperature and high concentration, the separated sulfuric acid flows into the sulfuric acid concentration section, hydrogen fluoride steam enters a hydrogen fluoride absorption tower, and hydrofluoric acid obtained after condensation and absorption is collected to a hydrofluoric acid buffer tank and is reserved for further treatment.
c. A sulfuric acid concentration section: and (3) sending the sulfuric acid from the stripping distillation tower to a sulfuric acid concentrator, concentrating to 94 wt% under the operating conditions of the pressure of 0.008MPa and the temperature of 190 ℃, continuously extracting one part of the sulfuric acid, sending the part of the sulfuric acid to a concentrated acid cooler, transferring the cooled concentrated sulfuric acid to a finished product acid tank by a finished product acid pump, and returning the other part of the sulfuric acid to a mixing stripping section to improve the concentration of the sulfuric acid in the concentrated acid cooler, wherein the operating pressure of the concentrated acid cooler is 0.008MPa, the shell-side temperature is 35 ℃, and the tube-side temperature is 110 ℃. And tail gas generated in the concentration process enters a tail gas condensing tower, and residual gas after condensation enters a gas washing tower and is discharged after the treatment reaches the standard.
After treatment according to this example, about 300 kg of 94 wt% concentrated sulfuric acid and 127 kg of 25 wt% hydrofluoric acid were produced per hour.
Other variations and modifications to the specific embodiments or examples described above will be apparent to those skilled in the art, given the benefit of this disclosure and the included scope of protection. Although the invention has been described in connection with specific embodiments or examples, which are intended to be illustrative rather than limiting, the present patent is accordingly not limited to the scope and effect of the several specific embodiments or examples described herein, nor is it limited to any other manner which is inconsistent with the progress in the art and which is achieved by the present invention.
Claims (7)
1. A safe and energy-saving purification treatment process of sulfuric acid containing fluorine is characterized by comprising a preheating evaporation section, a mixing removal section and a sulfuric acid concentration section;
the preheating evaporation section evaporates the raw material acid under vacuum condition to increase the concentration of sulfuric acid, the concentrated sulfuric acid is sent to the mixing removal section, and hydrogen fluoride steam generated in the evaporation process enters a hydrogen fluoride absorption tower;
the mixed removal section sends the sulfuric acid from the preheating evaporation section and the sulfuric acid from the sulfuric acid concentration section to a removal rectifying tower, hydrogen fluoride contained in the sulfuric acid is removed in a mixed manner, the sulfuric acid after defluorination is sent to the sulfuric acid concentration section, and hydrogen fluoride steam generated in the removal process enters a hydrogen fluoride absorption tower;
the sulfuric acid concentration section sends concentrated sulfuric acid from the mixing and removing section to a sulfuric acid concentrator, the concentration of the sulfuric acid is increased under the condition of high vacuum, one part of the obtained high-concentration sulfuric acid is continuously extracted out of the system, the other part of the obtained high-concentration sulfuric acid is sent back to the mixing and removing section to be mixed, and tail gas enters a tail gas condensation tower and a gas washing tower and is discharged after reaching the standard;
the concentration of the raw material acid is increased to 80-88 wt% in the preheating evaporation section;
the sulfuric acid concentration section increases the sulfuric acid concentration to 90-95 wt%;
the concentration of sulfuric acid in the mixed removal section is 88-90 wt%.
2. A safe and energy-saving sulfuric acid fluoride-containing purification process as set forth in claim 1, wherein said pre-heating evaporation stage comprises a pre-heater and a pre-evaporation evaporator.
3. A safe and energy-saving process for the purification treatment of fluorosulfuric acid as claimed in claim 2, wherein the preheater is made of silicon carbide, and the pre-evaporator is made of silicon carbide or steel sintered tetrafluoro.
4. The safe and energy-saving purification treatment process of sulfuric acid containing fluorine according to claim 1, wherein the raw material acid has a sulfuric acid concentration of 30 to 40 wt% and a hydrogen fluoride concentration of 10 to 20 wt%.
5. A safe and energy-saving purification treatment process of sulfuric acid containing fluorine according to claim 1, wherein the hydrogen fluoride absorption tower converts hydrogen fluoride into hydrofluoric acid by condensation absorption.
6. A safe and energy-saving process for the purification treatment of fluorosulfuric acid as claimed in claim 1, wherein the material of said dephlegmation and rectification column is steel sintered tetrafluoro.
7. A safe and energy-saving purification treatment process of sulfuric acid containing fluorine according to claim 1, wherein the sulfuric acid concentrator is made of silicon carbide.
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| CN102424367A (en) * | 2011-09-20 | 2012-04-25 | 六九硅业有限公司 | Fluorine-containing sulfuric acid separation concentration device and separation concentration method |
| US20120230906A1 (en) * | 2011-03-08 | 2012-09-13 | Trinapco, Inc. | Method of making fluorosulfonylamine |
| CN102923664A (en) * | 2012-11-27 | 2013-02-13 | 福州大学 | Method for producing hydrogen fluoride by virtue of gas-solid-liquid associative reaction method |
| CN105601012A (en) * | 2015-12-23 | 2016-05-25 | 韦建初 | Method for treating acid-containing waste liquid by condensation and distillation purification |
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|---|---|---|---|---|
| US20120230906A1 (en) * | 2011-03-08 | 2012-09-13 | Trinapco, Inc. | Method of making fluorosulfonylamine |
| CN102424367A (en) * | 2011-09-20 | 2012-04-25 | 六九硅业有限公司 | Fluorine-containing sulfuric acid separation concentration device and separation concentration method |
| CN102923664A (en) * | 2012-11-27 | 2013-02-13 | 福州大学 | Method for producing hydrogen fluoride by virtue of gas-solid-liquid associative reaction method |
| CN105601012A (en) * | 2015-12-23 | 2016-05-25 | 韦建初 | Method for treating acid-containing waste liquid by condensation and distillation purification |
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| Title |
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| 废硫酸回收新工艺;杨永福等;《环境工程》;20090630;第27卷(第3期);第108-109页 * |
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