CN109437108A - A kind of waste acidity recovery 26%-28% hydrogen chloride new process - Google Patents
A kind of waste acidity recovery 26%-28% hydrogen chloride new process Download PDFInfo
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- CN109437108A CN109437108A CN201811398983.3A CN201811398983A CN109437108A CN 109437108 A CN109437108 A CN 109437108A CN 201811398983 A CN201811398983 A CN 201811398983A CN 109437108 A CN109437108 A CN 109437108A
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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
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0712—Purification ; Separation of hydrogen chloride by distillation
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Abstract
The present invention relates to a kind of hydrogen chloride recovery process, more particularly to a kind of waste acidity recovery 26%-28% hydrogen chloride new process, it is passed through in stripper together with including the following steps: spent acid and the dense calcium chloride water after flash-evaporation dehydration via feed inlet, HCl steam is obtained after stripping column distillation, and it is discharged by the steam (vapor) outlet of stripper, into condenser system, remaining solution is discharged via the liquid outlet of the first stripper, into flash-evaporation dehydration step, compared with prior art, the beneficial effects of the present invention are: waste acid liquor and the solution Jing Guo flash-evaporation dehydration step enter stripper together, and HCl steam is formed by distillation, HCl steam is by dilution, condensation and demisting form dry HCl gas, it is conveyed, dilute hydrochloric acid will not be generated in removal process of the present invention, and the HCl gas of recycling is more succinct.
Description
Technical field
The present invention relates to a kind of hydrogen chloride recovery process, and in particular to a kind of new work of waste acidity recovery 26%-28% hydrogen chloride
Skill.
Background technique
The materials such as steel or equipment are cleaned with hydrochloric acid can generate the very high waste hydrochloric acid of a large amount of iron-content.These hydrochloric acid iron content
Height, concentration is low, lacks industrial application value.And it will cause serious pollution as direct discharging of waste water.Harmless treatment
It is again relatively high to neutralize cost, is always the problem of some enterprises.It can be by simple treatment process, under the conditions of comparatively gentle
These spent acid are handled, the technical grade concentrated hydrochloric acid of larger commercial value is obtained, chemical system are needed to the chlorination solved
The recycling of hydrogen and the purification of waste hydrochloric acid this common problem.
In Chemical Manufacture especially organic chlorides (or intermediate products) production, often generated with by-product hydrogen chloride.Work
The method for handling by-product hydrogen chloride in industry has: 31% hydrochloric acid is absorbed as with water, for other productions or as by-product hydrochloric acid
Sale；With azeotropic dilute hydrochloric acid (wherein, the mass fraction 18.5%~20% of HCl) cyclic absorption, stripped hydrogen chloride dry out is used again
In other productions (such as carbide VCM)；Hydrogen chloride (such as F22 production, day Bender are separated to obtain using dry method in production technology
Mountain and France's ATOCHEM methane chloride production process) it is re-used as industrial chemicals.
But some production technologies inevitably result from a large amount of dilute hydrochloric acid, especially there is chlorine in reaction generation water again
Change the occasion of hydrogen.
Therefore, a kind of new waste acidity recovery hydrogen chloride technique is developed, not only there is urgent researching value, it may have good
Economic benefit and commercial application potentiality, where this power exactly of the invention being accomplished and basis.
Summary of the invention
In order to overcome the defect of the prior art as indicated above, the present inventor has made intensive studies this, is paying
After a large amount of creative works, so as to complete the present invention.
Specifically, the technical problems to be solved by the present invention are: to provide a kind of waste acidity recovery 26%-28% hydrogen chloride new
Technique, to solve the technical issues of generating a large amount of dilute hydrochloric acid in existing chlorination hydrogen recovery process.
To achieve the above object, the invention provides the following technical scheme:
A kind of waste acidity recovery 26%-28% hydrogen chloride new process, includes the following steps:
(1) it distills
Spent acid and the dense calcium chloride water after flash-evaporation dehydration via feed inlet together be passed through in stripper, steamed through stripper
HCl steam is obtained after evaporating, and is discharged by the steam (vapor) outlet of stripper, and into condenser system, remaining solution is via the first stripping
The liquid outlet of tower is discharged, into flash-evaporation dehydration step；
(2) flash-evaporation dehydration
Stripper circulation is passed through again after reboiler boils via the solvent portions that stripper liquid outlet is discharged, it is another
Part solution is passed through in flash tank, and is mixed with the calcium chloride solution in flash tank and carried out dehydration by evaporation, the steam in flash tank
It is discharged by gas outlet, into waste gas system, the part solution in flash tank, which enters in flash tank evaporator, to be evaporated, then is followed
Ring is passed through in flash tank, and another part solution enters in the stripper in distilation steps via pipeline and calcium chloride solution pump；
(3) exhaust-gas treatment
The exhaust gas of flash tank gas outlet discharge enters in lime set tank by off-gas condenser, and the waste liquid of formation passes through lime set tank
Liquid outlet discharge；
(4) it dilutes
Thinning tank, the upper end of the thinning tank are entered by inlet by the HCl steam that the steam (vapor) outlet of stripper is discharged
Air inlet is passed through the HCl steam that degree is 10%-15%, enters condensing steps after the mixing of two steam；
(5) it condenses
The HCl steam being discharged by thinning tank steam (vapor) outlet is cooling by condensed in two stages, into demisting step；
(6) demisting
It is passed through in freezing demister by the cooling HCl steam of two-stage, is further dehydrated by low temperature demisting and obtains dry chlorine
Change hydrogen, during low temperature demisting, methanol hydrochlorination synthesis chloromethanes returns in stripper via pipeline.
In the present invention, as an improvement, the waste acid liquor being passed through in the distillation process is that degree is
The hydrochloric acid solution of 10%-15%.
In the present invention, as an improvement, the condensed in two stages includes being connected in series to stripping by connecting pipe
The first condenser and the second condenser of tower gas outlet, first condenser are passed through water and are condensed,
Second condenser is passed through ethylene glycol and is condensed.
In the present invention, as an improvement, it is 50%- that the HCl steam of the stripper discharge, which is degree,
55% steam.
In the present invention, as an improvement, the calcium chloride solution in the flash tank is that degree is 50%-
55% calcium chloride solution.
In the present invention, as an improvement, the freezing demister will enter HCl steam and be refrigerated to subzero 20 ° -25 °.
In the present invention, as an improvement, the chloromethanes returns in stripper to be repeated to distill, condense after distillation
And demisting step.
In the present invention, as an improvement, the tower bottom of the stripper is to absorb the water that dilute hydrochloric acid is brought into be formed
Dilute CaCl2Aqueous solution, the solution enter flash-evaporation dehydration in-process by the liquid outlet of stripper, the CaCl after concentration2Aqueous solution with
Hydrochloric acid enters in stripper together.
In the present invention, as an improvement, the cooling temperature of second condenser is subzero 20 ° -25 °.
In the present invention, as an improvement, in the exhaust-gas treatment process lime set tank liquid outlet be discharged waste liquid in HCl
Mass percent is less than 0.5%.
Compared with prior art, the beneficial effects of the present invention are:
(1) waste acid liquor and the solution Jing Guo flash-evaporation dehydration step enter stripper together, and form HCl steaming by distillation
Vapour, HCl steam form dry HCl gas by dilution, condensation and demisting, are conveyed, in removal process of the present invention
Dilute hydrochloric acid will not be generated, and the HCl gas recycled is more succinct.
(2) chloromethanes generated during low temperature demisting is returned in stripper by discharge tube, carries out secondary cycle,
Generation is recycled again generates hydrogen chloride steam.
Detailed description of the invention
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art are briefly described.In all the appended drawings, similar element
Or part is generally identified by similar appended drawing reference.In attached drawing, each element or part might not be drawn according to actual ratio.
Fig. 1 is process flow chart of the invention；
Specific embodiment
It is described in detail below in conjunction with embodiment of the attached drawing to technical solution of the present invention.Following embodiment is only used for
Clearly illustrate technical solution of the present invention, therefore be only used as example, and cannot be used as a limitation and limit protection model of the invention
It encloses.
Embodiment one: as shown in Figure 1, a kind of waste acidity recovery 26%-28% hydrogen chloride new process, includes the following steps:
(1) it distills
The spent acid that degree is 10% is passed through into pipeline with the dense calcium chloride water after flash-evaporation dehydration step
It is passed through in stripper via feed inlet, the HCl steam that degree is 50% is obtained after stripping column distillation, and by stripper
Steam (vapor) outlet discharge, into condenser system, the pressure of the stripper top is 0.15MPa, the temperature of the stripper bottom
Degree is 160 DEG C, remaining to absorb the mass percent that the water that dilute hydrochloric acid is brought into is formed as 40% dilute CaCl2Aqueous solution via
The liquid outlet of first stripper tower bottom is discharged, into flash-evaporation dehydration step；
(2) flash-evaporation dehydration
Dilute CaCl that mass percent via the discharge of stripper liquid outlet is 40%2Aqueous solution, a portion are passed through
Connecting pipe enters the reboiler being located on the outside of stripper, and reboiler is equipped with steam pipework, and steam pipework is to reboiler
The liquid heating of inner cavity makes its boiling, dilute CaCl after boiling2Aqueous solution is passed through stripper inner cavity, the HCl steam of formation again
It is discharged by steam (vapor) outlet, liquid circulation is discharged by stripper liquid outlet, does not enter another part mass percent of reboiler
For 40% dilute CaCl2Aqueous solution is passed through in flash tank, and the calcium chloride solution for being 50% with the degree in flash tank
Mixing carries out dehydration by evaporation, and the flashing pressure 0.05MPa in the flash tank, the interior water vapour evaporated of flash tank is by gas outlet
Discharge, into waste gas system, the part solution in flash tank enters in flash tank evaporator to be evaporated again, is followed again after dehydration
Ring is passed through in flash tank, the dense CaCl that flash tank bottom degree is 45% after evaporation2Aqueous solution is via pipeline and chlorination
Calcium solution pump enters in the stripper in distilation steps；
(3) exhaust-gas treatment
The exhaust gas of flash tank gas outlet discharge enters in lime set tank by off-gas condenser, and the waste liquid of formation passes through lime set tank
Liquid outlet is discharged, and HCl mass percent is less than 0.5% in the waste liquid that lime set tank liquid outlet is discharged in the exhaust-gas treatment process；
(4) it dilutes
Thinning tank, the upper end of the thinning tank are entered by inlet by the HCl steam that the steam (vapor) outlet of stripper is discharged
Air inlet is passed through the HCl steam that degree is 10%, the HCl steam and degree that the degree is 10%
Enter condensing steps to generate the HCl steam that degree is 30% after 50% HCl steam mixing；
(5) it condenses
The HCl steam that the degree being discharged by thinning tank steam (vapor) outlet is 30% by connecting pipe by being connected in series to
First condenser of stripper gas outlet and the condensation of the second condenser, first condenser is passed through water and condensed, and described the
Two condensers are passed through ethylene glycol and are condensed, and enter in demisting step after condensation；
(6) demisting
It is passed through in freezing demister by the cooling HCl steam of two-stage, is further dehydrated by subzero 20 ° of low temperature demisting
Dry hydrogen chloride is obtained, during low temperature demisting, methanol hydrochlorination synthesis chloromethanes returns in stripper via pipeline.
Embodiment two: a kind of waste acidity recovery 26%-28% hydrogen chloride new process includes the following steps:
(1) it distills
The spent acid that degree is 15% is passed through into pipeline with the dense calcium chloride water after flash-evaporation dehydration step
It is passed through in stripper via feed inlet, the HCl steam that degree is 55% is obtained after stripping column distillation, and by stripper
Steam (vapor) outlet discharge, into condenser system, the pressure of the stripper top is 0.15MPa, the temperature of the stripper bottom
Degree is 160 DEG C, remaining to absorb the mass percent that the water that dilute hydrochloric acid is brought into is formed as 45% dilute CaCl2Aqueous solution via
The liquid outlet of first stripper tower bottom is discharged, into flash-evaporation dehydration step；
(2) flash-evaporation dehydration
Dilute CaCl that mass percent via the discharge of stripper liquid outlet is 45%2Aqueous solution, a portion are passed through
Connecting pipe enters the reboiler being located on the outside of stripper, and reboiler is equipped with steam pipework, and steam pipework is to reboiler
The liquid heating of inner cavity makes its boiling, dilute CaCl after boiling2Aqueous solution is passed through stripper inner cavity, the HCl steam of formation again
It is discharged by steam (vapor) outlet, liquid circulation is discharged by stripper liquid outlet, does not enter another part mass percent of reboiler
For 45% dilute CaCl2Aqueous solution is passed through in flash tank, and the calcium chloride solution for being 50% with the degree in flash tank
Mixing carries out dehydration by evaporation, and the flashing pressure 0.05MPa in the flash tank, the interior water vapour evaporated of flash tank is by gas outlet
Discharge, into waste gas system, the part solution in flash tank enters in flash tank evaporator to be evaporated again, is followed again after dehydration
Ring is passed through in flash tank, the dense CaCl that flash tank bottom degree is 55% after evaporation2Aqueous solution is via pipeline and chlorination
Calcium solution pump enters in the stripper in distilation steps；
(3) exhaust-gas treatment
The exhaust gas of flash tank gas outlet discharge enters in lime set tank by off-gas condenser, and the waste liquid of formation passes through lime set tank
Liquid outlet is discharged, and HCl mass percent is less than 0.5% in the waste liquid that lime set tank liquid outlet is discharged in the exhaust-gas treatment process；
(4) it dilutes
Thinning tank, the upper end of the thinning tank are entered by inlet by the HCl steam that the steam (vapor) outlet of stripper is discharged
Air inlet is passed through the HCl steam that degree is 15%, the HCl steam and degree that the degree is 10%
Enter condensing steps to generate the HCl steam that degree is 30% after 55% HCl steam mixing；
(5) it condenses
The HCl steam that the degree being discharged by thinning tank steam (vapor) outlet is 30% by connecting pipe by being connected in series to
First condenser of stripper gas outlet and the condensation of the second condenser, first condenser is passed through water and condensed, and described the
Two condensers are passed through ethylene glycol and are condensed, and enter in demisting step after condensation；
(6) demisting
It is passed through in freezing demister by the cooling HCl steam of two-stage, is further dehydrated by subzero 25 ° of low temperature demisting
Dry hydrogen chloride is obtained, during low temperature demisting, methanol hydrochlorination synthesis chloromethanes returns in stripper via pipeline.
Embodiment three: a kind of waste acidity recovery 26%-28% hydrogen chloride new process includes the following steps:
(1) it distills
The spent acid that degree is 13% is passed through into pipeline with the dense calcium chloride water after flash-evaporation dehydration step
It is passed through in stripper via feed inlet, the HCl steam that degree is 53% is obtained after stripping column distillation, and by stripper
Steam (vapor) outlet discharge, into condenser system, the pressure of the stripper top is 0.15MPa, the temperature of the stripper bottom
Degree is 160 DEG C, remaining to absorb the mass percent that the water that dilute hydrochloric acid is brought into is formed as 42.5% dilute CaCl2Aqueous solution warp
It is discharged by the liquid outlet of the first stripper tower bottom, into flash-evaporation dehydration step；
(2) flash-evaporation dehydration
Dilute CaCl that mass percent via the discharge of stripper liquid outlet is 42.5%2Aqueous solution, a portion warp
It crosses connecting pipe and enters the reboiler being located on the outside of stripper, reboiler is equipped with steam pipework, and steam pipework is to reboiling
The liquid heating of device inner cavity makes its boiling, dilute CaCl after boiling2Aqueous solution is passed through stripper inner cavity again, and the HCl of formation steams
Vapour is discharged by steam (vapor) outlet, and liquid circulation is discharged by stripper liquid outlet, does not enter another part quality percentage of reboiler
Than dilute CaCl for 42.5%2Aqueous solution is passed through in flash tank, and the calcium chloride for being 47% with the degree in flash tank
Solution mixing carries out dehydration by evaporation, and the flashing pressure 0.05MPa in the flash tank, the interior water vapour evaporated of flash tank is by going out
Port discharge, into waste gas system, the part solution in flash tank enters in flash tank evaporator to be evaporated again, after dehydration
Recycling is passed through in flash tank, the dense CaCl that flash tank bottom degree is 53% after evaporation2Aqueous solution via pipeline and
Calcium chloride solution pump enters in the stripper in distilation steps；
(3) exhaust-gas treatment
The exhaust gas of flash tank gas outlet discharge enters in lime set tank by off-gas condenser, and the waste liquid of formation passes through lime set tank
Liquid outlet is discharged, and HCl mass percent is less than 0.5% in the waste liquid that lime set tank liquid outlet is discharged in the exhaust-gas treatment process；
(4) it dilutes
Thinning tank, the upper end of the thinning tank are entered by inlet by the HCl steam that the steam (vapor) outlet of stripper is discharged
Air inlet is passed through the HCl steam that degree is 13%, the HCl steam and degree that the degree is 13%
Enter condensing steps to generate the HCl steam that degree is 32.5% after 52% HCl steam mixing；
(5) it condenses
Passed through by the HCl steam that the degree that thinning tank steam (vapor) outlet is discharged is 32.5% and is connected by connecting pipe
It is condensed to the first condenser of stripper gas outlet and the second condenser, first condenser is passed through water and is condensed, described
Second condenser is passed through ethylene glycol and is condensed, and enters in demisting step after condensation；
(6) demisting
It is passed through in freezing demister by the cooling HCl steam of two-stage, is further dehydrated by subzero 23 ° of low temperature demisting
Dry hydrogen chloride is obtained, during low temperature demisting, methanol hydrochlorination synthesis chloromethanes returns in stripper via pipeline.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme should all cover within the scope of the claims and the description of the invention.
Claims (10)
1. a kind of waste acidity recovery 26%-28% hydrogen chloride new process, which comprises the steps of:
(1) it distills
Spent acid and the dense calcium chloride water after flash-evaporation dehydration via feed inlet together be passed through in stripper, after stripping column distillation
HCl steam is obtained, and is discharged by the steam (vapor) outlet of stripper, into condenser system, remaining solution is via the first stripper
Liquid outlet discharge, into flash-evaporation dehydration step；
(2) flash-evaporation dehydration
Stripper circulation, another part are passed through again after reboiler boils via the solvent portions that stripper liquid outlet is discharged
Solution is passed through in flash tank, and is mixed with the calcium chloride solution in flash tank and carried out dehydration by evaporation, and the steam in flash tank passes through
Gas outlet discharge, into waste gas system, the part solution in flash tank, which enters in flash tank evaporator, to be evaporated, and recycling is logical
Enter in flash tank, another part solution enters in the stripper in distilation steps via pipeline and calcium chloride solution pump；
(3) exhaust-gas treatment
The exhaust gas of flash tank gas outlet discharge enters in lime set tank by off-gas condenser, and the waste liquid of formation goes out liquid by lime set tank
Mouth discharge；
(4) it dilutes
Thinning tank, the upper end air inlet of the thinning tank are entered by inlet by the HCl steam that the steam (vapor) outlet of stripper is discharged
Mouth is passed through the HCl steam that degree is 10%-15%, enters condensing steps after the mixing of two steam；
(5) it condenses
The HCl steam being discharged by thinning tank steam (vapor) outlet is cooling by condensed in two stages, into demisting step；
(6) demisting
It is passed through in freezing demister by the cooling HCl steam of two-stage, is further dehydrated by low temperature demisting and obtains dry hydrogen chloride,
During low temperature demisting, methanol hydrochlorination synthesis chloromethanes returns in stripper via pipeline.
2. a kind of waste acidity recovery 26%-28% hydrogen chloride new process according to claim 1, it is characterised in that: the steaming
The waste acid liquor being passed through during evaporating is the hydrochloric acid solution that degree is 10%-15%.
3. a kind of waste acidity recovery 26%-28% hydrogen chloride new process according to claim 2, it is characterised in that: described two
Grade condensation includes the first condenser and the second condenser that stripper gas outlet is connected in series to by connecting pipe, first condensation
Device is passed through water and is condensed, and second condenser is passed through ethylene glycol and is condensed.
4. a kind of waste acidity recovery 26%-28% hydrogen chloride new process according to claim 1, it is characterised in that: the vapour
The HCl steam of stripper discharge is the steam that degree is 50%-55%.
5. a kind of waste acidity recovery 26%-28% hydrogen chloride new process according to claim 2, it is characterised in that: the sudden strain of a muscle
Calcium chloride solution in steaming pot is the calcium chloride solution that degree is 50%-55%.
6. a kind of waste acidity recovery 26%-28% hydrogen chloride new process according to claim 2, it is characterised in that: described cold
Subzero 20 ° -25 ° will be refrigerated into HCl steam by freezing demister.
7. a kind of waste acidity recovery 26%-28% hydrogen chloride new process according to claim 2, it is characterised in that: the chlorine
Methane, which returns in stripper, to be repeated to distill after distillation, condense and demisting step.
8. a kind of waste acidity recovery 26%-28% hydrogen chloride new process according to claim 2, it is characterised in that: the vapour
The tower bottom of stripper is to absorb dilute CaCl that the water that dilute hydrochloric acid is brought into is formed2Aqueous solution, the solution go out liquid by stripper
Mouth enters flash-evaporation dehydration in-process, the CaCl after concentration2Aqueous solution enters in stripper together with hydrochloric acid.
9. a kind of waste acidity recovery 26%-28% hydrogen chloride new process according to claim 3, it is characterised in that: described
The cooling temperature of two condensers is subzero 20 ° -25 °.
10. a kind of waste acidity recovery 26%-28% hydrogen chloride new process according to claim 2, it is characterised in that: described useless
HCl mass percent is less than 0.5% in the waste liquid that lime set tank liquid outlet is discharged in gas disposal process.
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| CN201811398983.3A CN109437108A (en) | 2018-11-22 | 2018-11-22 | A kind of waste acidity recovery 26%-28% hydrogen chloride new process |
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| CN201811398983.3A CN109437108A (en) | 2018-11-22 | 2018-11-22 | A kind of waste acidity recovery 26%-28% hydrogen chloride new process |
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Cited By (1)
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| CN110921630A (en) * | 2019-12-09 | 2020-03-27 | 北京诺维新材科技有限公司 | Method for preparing hydrogen chloride by resolving hydrochloric acid |
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