CN102249191A - Method and system for recycling waste fluorinated acid - Google Patents
Method and system for recycling waste fluorinated acid Download PDFInfo
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- CN102249191A CN102249191A CN 201110105154 CN201110105154A CN102249191A CN 102249191 A CN102249191 A CN 102249191A CN 201110105154 CN201110105154 CN 201110105154 CN 201110105154 A CN201110105154 A CN 201110105154A CN 102249191 A CN102249191 A CN 102249191A
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- supporting mass
- fluoridizing
- spent acid
- body skin
- production well
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Abstract
The invention provides a method for recycling waste fluorinated acid. In the method, hydrogen fluoride is recovered without secondary pollution. The method is characterized in that the waste fluorinated acid is distributed on the external surface of a supporting body at the temperature over 160 degrees; the supporting body is wrapped in a closed shell; and an upper vent hole is formed on the upper part of the shell corresponding to the supporting body, and the hydrogen fluoride and water vapor are led to a collecting unit via the upper vent hole so as to collect the hydrogen fluoride.
Description
Technical field
The present invention relates to fluoridize the processing technology field of spent acid, be specially a kind of method of fluoridizing the spent acid recycling, the present invention also provides the system of fluoridizing the spent acid recycling.
Background technology
Fluoridize spent acid, be arylamine to be carried out diazonium salt with anhydrous hydrogen fluoride decompose the synthetic spent acid that produces in the aromatic hydrocarbons process of fluoridizing, its main component is: hydrogen fluoride, water, sodium bifluoride, organism etc., prior art is to fluoridizing being treated to of spent acid: sulfuric acid or sulphur trioxide are blended into fluoridize in the spent acid, again through the distillation with hydrogen fluoride flash to gaseous state then condensation obtain more purified hydrogen fluoride, this treatment process, produce and the sulfur waste acid of fluoridizing the intimate equivalent of spent acid, and its composition is not limited to sulfur waste acid, complicated component, be difficult for handling, formed secondary pollution.
Summary of the invention
At the problems referred to above, the invention provides a kind of method of fluoridizing the spent acid recycling, it is reclaiming the hydrofluoric while, can not produce secondary pollution.
A kind of method of fluoridizing the spent acid recycling, it comprises fluoridizes spent acid, it is characterized in that: the described spent acid of fluoridizing is distributed in hull-skin temperature and is higher than on 160 ℃ the outside surface of supporting mass, described supporting mass is wrapped in the body skin of sealing, the corresponding body skin of described supporting mass top has the top production well, and hydrogen fluoride, water vapour lead to collection device by described top production well collects hydrogen fluoride.
It is further characterized in that: the solid grain thing of the outside surface of the described supporting mass of scraper scraping, by the solid grain thing relief outlet discharge on the body skin of the correspondence of the described solid grain thing scraping under by placing described supporting mass below;
The surface temperature of the outside surface of described supporting mass is specially 160 ℃～300 ℃;
Hydrogen fluoride by described top production well is respectively through being used for the synthetic aromatic hydrocarbons of fluoridizing of circulation after condensing works, the condensation of time condensation device;
The temperature at a described condensing works top is 70 ℃～100 ℃, and its internal condensation agent is a water; The temperature at described time condensation device top is 0 ℃～20 ℃, and its inner condensing agent is a chilled brine.
Fluoridize the system of spent acid recycling, it comprises the material sparger, it is characterized in that: supporting mass is positioned at body skin inside, described supporting mass internal communication heating plant, the outside surface towards described supporting mass is passed behind the described body skin in the outlet of described material sparger, the top of described body skin is provided with the top production well, and described top production well connects outside collection device.
It is further characterized in that: the correspondence of the outside surface of described supporting mass is furnished with scraper, and described scraper contacts the outside surface of described supporting mass; The bottom of described body skin is provided with spiral conveyer, and the bottom of described body skin has solid grain thing outlet orifice, and described spiral conveyer leads to described solid grain thing outlet orifice;
Described supporting mass is specially cylinder, and described drum sleeve is loaded on main shaft, and described main shaft is loaded on the inside of described body skin, and described heating plant is communicated with the inside of described cylinder by heating tube;
Described supporting mass is specially the worktable of horizontal translation, and the bottom cooperation of described worktable is equipped with guide rail, and described guide rail is positioned at described body skin inside, and described heating plant is communicated with described worktable inside by heating tube;
Described collection device comprises condensing works, and described condensing works specifically comprises primary condenser, after-condenser, and described top production well, primary condenser, after-condenser connect successively.
After adopting method of the present invention, fluoridize the hydrogen fluoride in the spent acid, water is direct gasification in the environment more than 160 ℃, sodium bifluoride decomposes generation hydrogen fluoride and Sodium Fluoride in the environment more than 160 ℃, hydrogen fluoride direct gasification wherein, hydrogen fluoride like this, water vapour just is located away from the body skin of sealing by the top production well, enter condensing works, reclaim hydrofluoric purpose by reaching behind the condensing works afterwards, in addition, organism is directly carbonization in the environment more than 160 ℃, and the Sodium Fluoride that is produced all can not produce secondary pollution, so it is reclaiming the hydrofluoric while, can not produce secondary pollution.
Description of drawings
Fig. 1 is a structural representation of fluoridizing system's embodiment one of spent acid recycling of the present invention;
Fig. 2 is a structural representation of fluoridizing system's embodiment two of spent acid recycling of the present invention.
Embodiment
A kind of method of fluoridizing the spent acid recycling,
Specific embodiment one: fluoridizing spent acid, to be distributed in surface temperature be on 160 ℃ the supporting mass of outside surface, supporting mass is wrapped in the body skin of sealing, the corresponding body skin of supporting mass top has the top production well, hydrogen fluoride, water vapour are collected purified hydrogen fluoride after leading to collection device by the top production well, the solid grain thing of the outside surface of scraper scraping supporting mass is discharged by the solid grain thing relief outlet that the spiral conveyer that places the supporting mass below is delivered to the body skin bottom by the solid grain thing under the scraping;
Hydrogen fluoride by the top production well is respectively through being used for the synthetic aromatic hydrocarbons of fluoridizing of circulation after condensing works, the condensation of time condensation device; The temperature at a condensing works top is 70 ℃, and its internal condensation agent is a water; The temperature at time condensation device top is 0 ℃, and its inner condensing agent is a chilled brine.
Specific embodiment two: fluoridizing spent acid, to be distributed in surface temperature be on 300 ℃ the supporting mass of outside surface, supporting mass is wrapped in the body skin of sealing, the corresponding body skin of supporting mass top has the top production well, hydrogen fluoride, water vapour are collected purified hydrogen fluoride after leading to collection device by the top production well, the solid grain thing of the outside surface of scraper scraping supporting mass is discharged by the solid grain thing relief outlet that the spiral conveyer that places the supporting mass below is delivered to the body skin bottom by the solid grain thing under the scraping;
Hydrogen fluoride by the top production well is respectively through being used for the synthetic aromatic hydrocarbons of fluoridizing of circulation after condensing works, the condensation of time condensation device; The temperature at a condensing works top is 100 ℃, and its internal condensation is a water; The temperature at time condensation device top is 20 ℃, and its inner condensing agent is a chilled brine.
Specific embodiment three: fluoridizing spent acid, to be distributed in surface temperature be on 230 ℃ the supporting mass of outside surface, supporting mass is wrapped in the body skin of sealing, the corresponding body skin of supporting mass top has the top production well, hydrogen fluoride, water vapour are collected purified hydrogen fluoride after leading to condensing works by the top production well, the solid grain thing of the outside surface of scraper scraping supporting mass is discharged by the solid grain thing relief outlet that the spiral conveyer that places the supporting mass below is delivered to the body skin bottom by the solid grain thing under the scraping;
Hydrogen fluoride by the top production well is respectively through being used for the synthetic aromatic hydrocarbons of fluoridizing of circulation after condensing works, the condensation of time condensation device; The temperature at a condensing works top is 85 ℃, and its internal condensation agent is a water; The temperature at time condensation device top is 10 ℃, and its inner condensing agent is a chilled brine.
Solid grain thing among three embodiment comprises organic carbide, Sodium Fluoride.
Fluoridize the system of spent acid recycling,
Embodiment one, see Fig. 1, it comprises material sparger 1, cylinder 2 is positioned at body skin 3 inside, the outside surface of body skin 3 backs towards cylinder 2 passed in the outlet of material sparger 1, cylinder 2 is set in main shaft 4, and main shaft 4 is loaded on the inside of body skin 3, and heating plant 5 is communicated with the inside of cylinder 2 by heating tube 6; The top of body skin 3 is provided with top production well 7, and top production well 7 connects outside condensing works.The outside surface correspondence of cylinder 2 is furnished with scraper 8, the outside surface of scraper 8 contact cylinders 2; Scraper 8 is loaded on body skin 3 inside; The bottom of body skin 3 is provided with spiral conveyer 10, and the bottom of body skin 3 has solid grain thing outlet orifice 9, and spiral conveyer 10 leads to solid grain thing outlet orifice 9; Condensing works specifically comprises primary condenser 11, after-condenser 12, top production well 7 connects the lower inlet of primary condenser 11, hydrofluoric acid is flowed out in the sidepiece outlet of primary condenser 11, the top exit of primary condenser 11 connects the lower inlet of after-condenser 12, the side opening of after-condenser 12 is discharged and can be directly used in the synthetic hydrogen fluoride of fluoridizing aromatic hydrocarbons of circulation, and the top exit of after-condenser 12 is connected with spray equipment 13.
Embodiment two, see Fig. 2, it comprises material sparger 1, the worktable 14 of horizontal translation is positioned at body skin 3 inside, the upper surface of body skin 3 backs towards the worktable 14 of horizontal translation passed in the outlet of material sparger 1, the bottom cooperation of worktable 14 is equipped with guide rail 15, and guide rail 15 is positioned at body skin 3 inside, and heating plant 5 is communicated with the inside of worktable 14 by heating tube 6; The top of body skin 3 is provided with top production well 7, and top production well 7 connects outside condensing works.The upper surface correspondence of worktable 14 be furnished with scraper 8 ', the upper surface of scraper 8 ' contact worktable 14, scraper 8 ' be loaded on body skin 3 inside; The bottom of body skin 3 is provided with spiral conveyer 10, and the bottom of body skin 3 has solid grain thing outlet orifice 9, and spiral conveyer 10 leads to solid grain thing outlet orifice 9; Condensing works specifically comprises primary condenser 11, after-condenser 12, and top production well 7, primary condenser 11, after-condenser 12 connect successively.Top production well 7 connects the lower inlet of primary condenser 11, hydrofluoric acid is flowed out in the sidepiece outlet of primary condenser 11, the top exit of primary condenser 11 connects the lower inlet of after-condenser 12, the side opening of after-condenser 12 connects rectifying tower 16, the top exit of after-condenser 12 is connected with spray equipment 13, and the top exit of rectifying tower 16 is finally discharged anhydrous hydrogen fluoride.
Scraper 8 ' thickness little, can not disturb material sparger 1 to distribute and fluoridize spent acid to the upper surface of worktable 14.
Its principle of work is as follows: fluoridize spent acid is distributed in supporting mass (cylinder 2 or worktable 14) by material sparger 1 outside surface, because the temperature of the outside surface of supporting mass is higher than 160 ℃, hydrogen fluoride, water is direct gasification in the environment more than 160 ℃, sodium bifluoride decomposes generation hydrogen fluoride and Sodium Fluoride in the environment more than 160 ℃, hydrogen fluoride direct gasification wherein, hydrogen fluoride like this, water vapour just is located away from the body skin 3 of sealing by the top production well, enter condensing works, reclaim hydrofluoric purpose by reaching behind the condensing works afterwards, wherein the tail gas of 13 pairs of discharges of the spray equipment that top exit connected of after-condenser 12 sprays, and has obtained water hydrofluoric acid thereby collect; The temperature at primary condenser 11 tops is 70 ℃～100 ℃, and condensing agent is a water, and after hydrogen fluoride entered primary condenser 11, water vapour combined with small part hydrogen fluoride, forms hydrofluoric acid, and hydrofluoric acid flows out from the sidepiece outlet of primary condenser 11; All the other most hydrogen fluoride rise, flow into the lower inlet of after-condenser 12 from the top exit of primary condenser 11, the temperature at after-condenser 12 tops is 0 ℃～20 ℃, condensing agent is a chilled brine, be condensed hydrogen fluoride discharge from the side opening of after-condenser 12, can be directly used in the synthetic hydrogen fluoride of fluoridizing aromatic hydrocarbons of circulation, be not condensed hydrogen fluoride flow out from the top exit of after-condenser 12; In order to collect more purified hydrogen fluoride, also can connect rectifying tower 16 at the side opening of after-condenser 12, the top exit of rectifying tower 16 is finally discharged anhydrous hydrogen fluoride.In addition, organism carbide after the direct carbonization in the environment more than 160 ℃ constitutes solid grain thing with the Sodium Fluoride that is produced, Gu the grain thing is distributed in the outside surface that contacts of fluoridizing waste liquid and supporting mass, afterwards by the scraper scraping, thereby the outside surface that breaks away from supporting mass, dropping enters spiral conveyer 10, finally is delivered to solid grain thing outlet orifice 9 by spiral conveyer 10 and is discharged from, and the solid grain thing that is discharged from is sent into the Sodium Fluoride that other processing machines are processed to form certain precision.To sum up, it need not to reclaim the hydrogen fluoride of fluoridizing in the spent acid with sulfuric acid, sulphur trioxide, has stopped a large amount of spent acid solutions and has produced, and can not produce secondary pollution, security is good; And the hydrogen fluoride circulation that can adopt recovery is used for synthesizing fluoridizes aromatic hydrocarbons, has reduced the cost of product; Owing to adopted solid grain thing recycling module, can fully reclaim Sodium Fluoride, the resource utilization maximization.
Claims (10)
1. method of fluoridizing the spent acid recycling, it comprises fluoridizes spent acid, it is characterized in that: the described spent acid of fluoridizing is distributed in hull-skin temperature and is higher than on 160 ℃ the outside surface of supporting mass, described supporting mass is wrapped in the body skin of sealing, the corresponding body skin of described supporting mass top has the top production well, and hydrogen fluoride, water vapour lead to collection device by described top production well collects hydrogen fluoride.
2. a kind of method of fluoridizing the spent acid recycling according to claim 1, it is characterized in that: the solid grain thing of the outside surface of the described supporting mass of scraper scraping, by the solid grain thing relief outlet discharge on the body skin of the correspondence of the described solid grain thing scraping under by placing described supporting mass below.
3. a kind of method of fluoridizing the spent acid recycling according to claim 1 is characterized in that: the surface temperature of the outside surface of described supporting mass is specially 160 ℃～300 ℃.
4. a kind of method of fluoridizing the spent acid recycling according to claim 1 is characterized in that: the hydrogen fluoride by described top production well is respectively through being used for the synthetic aromatic hydrocarbons of fluoridizing of circulation after condensing works, the condensation of time condensation device.
5. a kind of method of fluoridizing the spent acid recycling according to claim 4 is characterized in that: the temperature at a described condensing works top is 70 ℃～100 ℃, and its internal condensation agent is a water; The temperature at described time condensation device top is 0 ℃～20 ℃, and its inner condensing agent is a chilled brine.
6. fluoridize the system of spent acid recycling, it comprises the material sparger, it is characterized in that: supporting mass is positioned at body skin inside, described supporting mass internal communication heating plant, the outside surface towards described supporting mass is passed behind the described body skin in the outlet of described material sparger, the top of described body skin is provided with the top production well, and described top production well connects outside collection device.
7. system of fluoridizing the spent acid recycling according to claim 6 is characterized in that: the correspondence of the outside surface of described supporting mass is furnished with scraper, and described scraper contacts the outside surface of described supporting mass; The bottom of described body skin is provided with spiral conveyer, and the bottom of described body skin has solid grain thing outlet orifice, and described spiral conveyer leads to described solid grain thing outlet orifice.
8. system of fluoridizing the spent acid recycling according to claim 6, it is characterized in that: described supporting mass is specially cylinder, described drum sleeve is loaded on main shaft, and described main shaft is loaded on the inside of described body skin, and described heating plant is communicated with the inside of described cylinder by heating tube.
9. system of fluoridizing the spent acid recycling according to claim 6, it is characterized in that: described supporting mass is specially the worktable of horizontal translation, the bottom cooperation of described worktable is equipped with guide rail, described guide rail is positioned at described body skin inside, and described heating plant is communicated with described worktable inside by heating tube.
10. according to the described system of fluoridizing the spent acid recycling of the arbitrary claim of claim 6 to 9, it is characterized in that: described collection device comprises condensing works, described condensing works specifically comprises primary condenser, after-condenser, and described top production well, primary condenser, after-condenser connect successively.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110105154 CN102249191A (en) | 2011-04-26 | 2011-04-26 | Method and system for recycling waste fluorinated acid |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110105154 CN102249191A (en) | 2011-04-26 | 2011-04-26 | Method and system for recycling waste fluorinated acid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105800559A (en) * | 2014-12-30 | 2016-07-27 | 有研稀土新材料股份有限公司 | Hydrofluoric acid recycling device and hydrofluoric acid recycling method |
| CN113401916A (en) * | 2021-05-26 | 2021-09-17 | 大连鼎燕医药化工有限公司 | Waste utilization of substituted aromatic hydrocarbon hydrogen fluoride diazonium salt pyrolysis fluorination reaction |
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| CN1651338A (en) * | 2004-02-05 | 2005-08-10 | 黄健 | Production method of waste acid regeneration and by product ferrous chloride |
| CN201031140Y (en) * | 2007-01-08 | 2008-03-05 | 战玉柏 | Device for producing ultra-clear and high-purity |
| CN101218175A (en) * | 2005-04-10 | 2008-07-09 | 瑞科硅公司 | Production of polycrystalline silicon |
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2011
- 2011-04-26 CN CN 201110105154 patent/CN102249191A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1651338A (en) * | 2004-02-05 | 2005-08-10 | 黄健 | Production method of waste acid regeneration and by product ferrous chloride |
| CN101218175A (en) * | 2005-04-10 | 2008-07-09 | 瑞科硅公司 | Production of polycrystalline silicon |
| CN201031140Y (en) * | 2007-01-08 | 2008-03-05 | 战玉柏 | Device for producing ultra-clear and high-purity |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105800559A (en) * | 2014-12-30 | 2016-07-27 | 有研稀土新材料股份有限公司 | Hydrofluoric acid recycling device and hydrofluoric acid recycling method |
| CN105800559B (en) * | 2014-12-30 | 2018-03-16 | 有研稀土新材料股份有限公司 | The recycling device of hydrofluoric acid and the recycling method of hydrofluoric acid |
| CN113401916A (en) * | 2021-05-26 | 2021-09-17 | 大连鼎燕医药化工有限公司 | Waste utilization of substituted aromatic hydrocarbon hydrogen fluoride diazonium salt pyrolysis fluorination reaction |
| CN113401916B (en) * | 2021-05-26 | 2023-05-26 | 大连鼎燕医药化工有限公司 | Waste utilization of pyrolysis fluoro reaction of substituted aromatic hydrocarbon hydrogen fluoride diazonium salt |
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Application publication date: 20111123 |