CN104326442A - Recycling separation method and system for HF and H2SO4 mixed acid - Google Patents

Recycling separation method and system for HF and H2SO4 mixed acid Download PDF

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Publication number
CN104326442A
CN104326442A CN201410638269.2A CN201410638269A CN104326442A CN 104326442 A CN104326442 A CN 104326442A CN 201410638269 A CN201410638269 A CN 201410638269A CN 104326442 A CN104326442 A CN 104326442A
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water
bipolar membrane
membrane assembly
solution
separation method
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CN104326442B (en
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刘晨明
李志强
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Beijing Saike Kanglun Environmental Science & Technology Co Ltd
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Beijing Saike Kanglun Environmental Science & Technology Co Ltd
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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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/69—Sulfur trioxide; Sulfuric acid
    • C01B17/90—Separation; Purification

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)

Abstract

The invention discloses a recycling separation method for HF and H2SO4 mixed acid. The recycling separation method comprises the following steps: after adjusting pH to 5-7 with an alkali liquid in a pH adjusting tank, enabling the acid into a nano-filtration membrane module and intercepting and separating to obtain an F<->-containing salt solution and an SO4<2->-containing salt solution; respectively recycling HF and H2SO4 in double-pole membrane modules and simultaneously recycling the alkali liquid; returning the alkali liquid back to the pH adjusting tank to be used as an adjusting reagent; enabling residual output water of the two sets of double-pole membrane modules to respectively enter a concentration device to be further concentrated; returning the water back to the double-pole membrane module at the front end to be used as input water of a salt chamber; and discharging and recycling fresh water. According to the recycling separation method and system, the defects of a traditional HF and H2SO4 separation method that the energy consumption is great, the requirements on materials of equipment are high, the HF recycling rate is low, the operation is not safe and the like are mainly overcome; and the process has the advantages of low consumption, high HF recycling rate, simplicity and safety in operation and the like.

Description

A kind of HF and H 2sO 4the resource separation of mixing acid and system thereof
Technical field
The invention belongs to water treatment field, particularly relate to a kind of HF and H 2sO 4the separation method of mixing acid and system thereof.
Background technology
Often HF and H can be produced in Industrial processes 2sO 4mixing spent acid, due to HF and H 2sO 4often can not be used in combination, therefore in order to avoid the waste of resource, need to manage HF and H 2sO 4be separated.Tradition is separated HF and H 2sO 4method be mainly distillation method.
Distillation method mainly refers to by HF and H 2sO 4the difference of boiling point, by HF and H 2sO 4separate.HF is the acid of a kind of easy volatile, and its boiling point is 112.2 DEG C, by comparison, and H 2sO 4boiling point then much higher, be 338 DEG C, when to HF and H 2sO 4the heating of mixing spent acid time, HF first volatilizees because boiling point is lower, and it is cold solidifying or be pure HF solution after absorbing, thus realizes HF and H 2sO 4separately.The technical process of this method is simple, but energy consumption is very high, and the temperature in addition due to HF steam is higher, not easily condensation, and the rate of recovery of HF is lower and there is potential safety hazard.
Conventional espresso method has that energy consumption is large, the HF rate of recovery is low and the shortcoming such as potential safety hazard is large, in order to more environmental protection, more energy-conservation is separated HF and H 2sO 4, explore more effective HF and H 2sO 4the separation method of mixing spent acid is very urgent.
Summary of the invention
In order to solve traditional HF and H 2sO 4the energy expenditure of mixing spent acid separation method is large, the resource utilization rate of recovery is low and operate uneasy congruent problem, and the present invention proposes a kind of low consumption, safety coefficient is high and the resource utilization rate of recovery is high HF and H 2sO 4mixing spent acid separation method.
For reaching above-mentioned purpose, the present invention adopts following technical scheme:
A kind of HF and H 2sO 4the separation method of mixing acid, it comprises the steps:
(1) HF and H 2sO 4first mixing acid enter pH regulator pond, regulates pH to 5 ~ 7 with alkali lye;
Step (1) is the significant process of pre-treatment mixing spent acid, its objective is and acid is converted into salt, be beneficial to subsequent operations.The alkali lye regulating pH can be Ca (OH) 2or NaOH;
(2) enter nanofiltration membrane component from step (1) solution out and retain separation, obtain containing F -salts solution and containing SO 4 2-salts solution;
Step (2) is separated F -and SO 4 2-main process;
(3) from step (2) out containing F -salts solution enters first set Bipolar Membrane assembly to carry out acid-alkali regeneration and obtains HF solution and alkali lye 1, containing SO 4 2-salts solution enters the second cover Bipolar Membrane assembly to carry out acid-alkali regeneration and obtains H 2sO 4solution and alkali lye 2;
Step (3) reclaims HF, H 2sO 4with the main process of alkali lye;
(4) enter electrodialysis 1 from step (3) first set Bipolar Membrane assembly raffinate out or reverse osmosis 1 concentrates, dense water returns first set Bipolar Membrane assembly as the water inlet of salt room, fresh water qualified discharge or reuse; Overlap Bipolar Membrane assembly raffinate out from step (3) second and enter electrodialysis 2 or reverse osmosis 2 concentrates, dense water returns the second cover Bipolar Membrane assembly as the water inlet of salt room, fresh water qualified discharge or reuse;
Step (4) is the main process realizing effluent quality qualified discharge or reuse;
(5) step (1) is returned from step (3) alkali lye 1 out and alkali lye 2.
Step (5) reduces to consume, and realizes the significant process of resource circulation utilization.Can select to be enter electrodialysis or reverse osmosis according to its concentration level from Bipolar Membrane assembly fresh water out, if its concentration is higher, then enter electrodialysis, otherwise if its concentration is lower, then enter reverse osmosis.
Preferably PH to 7 is regulated with alkali lye in step (1).
A kind of system realizing described separation method, it comprises: PH equalizing tank, nanofiltration membrane component, two cover Bipolar Membrane assemblies, two cover concentrating uniies, described PH equalizing tank water outlet is connected with nanofiltration membrane component water-in, first water outlet of nanofiltration membrane component is connected with first set Bipolar Membrane assembly salt room water-in, second water outlet and second overlaps Bipolar Membrane assembly salt room water-in and is connected, and the raffinate outlet of first, second cover Bipolar Membrane assembly is connected with a concentrating unit respectively.
Described concentrating unit comprises electrodialysis and reverse osmosis;
Preferably, described concentrating unit is set to one or both in electrodialysis or reverse osmosis.
The alkali room water outlet of first, second cover Bipolar Membrane assembly described all returns PH equalizing tank as regulating agent, and HF solution and H are reclaimed in the water outlet of sour room respectively 2sO 4solution.
The dense water out of described concentrating unit all returns and is connected with the salt room water-in of its front end Bipolar Membrane assembly, and dense water is as the water inlet of salt room, and fresh water discharges or recycles.
Described HF and H 2sO 4in mixing acid, HF content is 0.5% ~ 50%, H 2sO 4content is 0.5% ~ 98%.
Accompanying drawing 1 is shown in the technical process of above-mentioned steps.
As optimal technical scheme, method of the present invention, HF and H described in step (1) 2sO 4the content of the HF in mixing acid is 0.5% ~ 50%, such as, be 1% ~ 10%, 5% ~ 20%, 10% ~ 30%, 20% ~ 45% etc., H 2sO 4content be 0.5% ~ 98%, be such as 1% ~ 10%, 5% ~ 20%, 10% ~ 30%, 20% ~ 45%, 40% ~ 65%, 50% ~ 80%, etc.HF and H of process of the present invention 2sO 4mixing acid does not have strict requirement, HF and H 2sO 4content can in a larger scope, therefore the scope of application of the present invention is very wide.
As optimal technical scheme, method of the present invention, for regulating the alkali lye of pH can be Ca (OH) in step (1) 2or NaOH, but consider the scale problems of subsequent film assembly, preferentially use NaOH.PH regulator to 5 ~ 7 of mixing acid, such as, be: 5,5.5,6,6.3,6.5 etc.
As optimal technical scheme, method of the present invention, from step (3) if first set Bipolar Membrane assembly raffinate salt concn is out higher in step (4), then preferentially enters electrodialysis process and concentrate, otherwise it is concentrated then to enter reverse osmosis process; From step (3) if the second cover Bipolar Membrane assembly raffinate salt concn is out higher, then preferentially enter electrodialysis process and concentrate, otherwise it is concentrated then to enter reverse osmosis process.
As optimal technical scheme, method of the present invention, comprises the steps:
(1) HF and H 2sO 4first mixing acid enter pH regulator pond 1, regulates pH=5 ~ 7 with NaOH;
(2) enter nanofiltration membrane component from step (1) solution out, obtain NaF solution and Na 2sO 4solution;
(3) enter first set Bipolar Membrane assembly from step (2) NaF solution out to carry out acid-alkali regeneration and obtain HF and NaOH solution 1, Na 2sO 4solution enters the second cover Bipolar Membrane assembly to carry out acid-alkali regeneration and obtains H 2sO 4with NaOH solution 2;
(4) from step (3) if first set Bipolar Membrane assembly raffinate salt concn is out higher, then enter electrodialysis process and concentrate, otherwise it is concentrated then to enter reverse osmosis process; From step (3) if the second cover Bipolar Membrane assembly raffinate salt concn is out higher, then enter electrodialysis process and concentrate, otherwise then enter reverse osmosis process and concentrate, one in electrodialysis or reverse osmosis can be set as required or two kinds or many groups use simultaneously.
(5) step (1) is returned from step (3) NaOH solution 1 out and NaOH solution 2.
compare with conventional art, the present invention has following beneficial effect:
1, effluent quality F of the present invention -and SO 4 2-stable content up to standard, can discharge or reuse;
2, consumption of the present invention is few, consumes except a small amount of alkali lye except running for the first time, follow-uply not only no longer consumes extra alkali, but also can reclaim the alkali lye that concentration is 0.5% ~ 10%, and the regeneration rate of alkali lye reaches more than 90%;
3, HF and H of the present invention 2sO 4the rate of recovery all reach more than 95%.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of separation method of the present invention.
Embodiment
For better the present invention being described, be convenient to understand technical scheme of the present invention, below the present invention is described in more detail.But following embodiment is only simple and easy example of the present invention, and do not represent or limit the scope of the present invention, protection scope of the present invention is as the criterion with claims.
embodiment 1
HF and H of certain factory 2sO 4mixing spent acid, the content of HF is 12%, H 2sO 4content be 26%.
(1) HF and H of 100L 2sO 4first mixing acid enter pH regulator pond 1, regulates pH=7 with 2%NaOH, obtains the solution that salt concn is 2.67%;
(2) solution being 2.67% from step (1) salt concn out enters nanofiltration membrane component, and producing water ratio is 50%, SO 4 2-rejection, more than 98.5%, obtains 2.1%NaF solution and 4%Na 2sO 4solution;
(3) enter first set Bipolar Membrane assembly from step (2) 2.1%NaF solution out to carry out acid-alkali regeneration and obtain 1.5% ~ 3%HF and 1% ~ 2%NaOH, 4%Na 2sO 4solution enters the second cover Bipolar Membrane assembly to carry out acid-alkali regeneration and obtains 1% ~ 5%H 2sO 4with 1% ~ 4%NaOH solution;
(4) enter reverse osmosis process from step (3) first set Bipolar Membrane assembly 0.2% ~ 1% raffinate out to concentrate, obtain 0.5% ~ 2.5% dense water returns first set Bipolar Membrane assembly, 0.0001% fresh water qualified discharge or reuse; Enter electrodialysis process from step (3) second cover Bipolar Membrane assembly 0.4% ~ 2% raffinate out to concentrate, obtain 1% ~ 4% dense water returns the second cover Bipolar Membrane assembly, 0.0001% fresh water qualified discharge or reuse.
(5) step (1) is returned from step (3) NaOH solution out.
embodiment 2
HF and H of certain factory 2sO 4mixing spent acid, the content of HF is 30%, H 2sO 4content be 25%.
(1) HF and H of 100L 2sO 4first mixing acid enter pH regulator pond 1, regulates pH=7 with 5%NaOH, obtains the solution that salt concn is 5.8%;
(2) solution being 5.8% from step (1) salt concn out enters nanofiltration membrane component, and producing water ratio is 60%, SO 4 2-rejection, more than 98.5%, obtains 6.2%NaF solution and 5.3%Na 2sO 4solution;
(3) enter first set Bipolar Membrane assembly from step (2) 6.2%NaF solution out to carry out acid-alkali regeneration and obtain 2% ~ 6%HF and 1% ~ 6%NaOH, 5.3%Na 2sO 4solution enters the second cover Bipolar Membrane assembly to carry out acid-alkali regeneration and obtains 2% ~ 5%H 2sO 4with 1% ~ 5%NaOH solution;
(4) enter electrodialysis process from step (3) first set Bipolar Membrane assembly 0.5% ~ 2.5% raffinate out to concentrate, obtain 1% ~ 5% dense water returns first set Bipolar Membrane assembly, 0.0001% fresh water qualified discharge or reuse; Enter electrodialysis process from step (3) second cover Bipolar Membrane assembly 0.5% ~ 3% raffinate out to concentrate, obtain 2% ~ 6% dense water returns the second cover Bipolar Membrane assembly, 0.0001% fresh water qualified discharge or reuse.
(5) step (1) is returned from step (3) NaOH solution out.
embodiment 3
HF and H of certain factory 2sO 4mixing spent acid, the content of HF is 15%, H 2sO 4content be 52%.
(1) HF and H of 100L 2sO 4first mixing acid enter pH regulator pond 1, regulates pH=7 with 8%NaOH, obtains the solution that salt concn is 10.6%;
(2) solution being 10.6% from step (1) salt concn out enters nanofiltration membrane component, and producing water ratio is 60%, SO 4 2-rejection, more than 98.5%, obtains 5.2%NaF solution and 18.8%Na 2sO 4solution;
(3) enter first set Bipolar Membrane assembly from step (2) 5.2%NaF solution out to carry out acid-alkali regeneration and obtain 2% ~ 5%HF and 1% ~ 5%NaOH, 18.8%Na 2sO 4solution enters the second cover Bipolar Membrane assembly to carry out acid-alkali regeneration and obtains 7% ~ 18%H 2sO 4with 5% ~ 15%NaOH solution;
(4) enter electrodialysis process from step (3) first set Bipolar Membrane assembly 0.5% ~ 2.5% raffinate out to concentrate, obtain 1% ~ 5% dense water returns first set Bipolar Membrane assembly, 0.0001% fresh water qualified discharge or reuse; Enter electrodialysis process from step (3) second cover Bipolar Membrane assembly 2% ~ 8% raffinate out to concentrate, obtain 5% ~ 15% dense water returns the second cover Bipolar Membrane assembly, 0.0001% fresh water qualified discharge or reuse.
(5) step (1) is returned from step (3) NaOH solution out.
Applicant states, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, namely do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.

Claims (7)

1. HF and H 2sO 4the separation method of mixing acid, it comprises the steps:
(1) HF and H 2sO 4first mixing acid enter pH regulator pond, regulates pH to 5 ~ 7 with alkali lye;
(2) enter nanofiltration membrane component from step (1) solution out and retain separation, obtain containing F -salts solution and containing SO 4 2-salts solution;
(3) from step (2) out containing F -salts solution enters first set Bipolar Membrane assembly to carry out acid-alkali regeneration and obtains HF solution and alkali lye 1, containing SO 4 2-salts solution enters the second cover Bipolar Membrane assembly to carry out acid-alkali regeneration and obtains H 2sO 4solution and alkali lye 2;
(4) enter electrodialysis 1 from step (3) first set Bipolar Membrane assembly raffinate out or reverse osmosis 1 concentrates, dense water returns first set Bipolar Membrane assembly as the water inlet of salt room, fresh water qualified discharge or reuse; Overlap Bipolar Membrane assembly raffinate out from step (3) second and enter electrodialysis 2 or reverse osmosis 2 concentrates, dense water returns the second cover Bipolar Membrane assembly as the water inlet of salt room, fresh water qualified discharge or reuse;
(5) step (1) is returned from step (3) alkali lye 1 out and alkali lye 2.
2. separation method as claimed in claim 1, is characterized in that, preferably regulates PH to 7 with alkali lye in step (1).
3. one kind realizes the system as weighed separation method as described in 1, it is characterized in that, it comprises: pH regulator pond, nanofiltration membrane component, two cover Bipolar Membrane assemblies, two cover concentrating uniies, described pH regulator pond water outlet is connected with nanofiltration membrane component water-in, first water outlet of nanofiltration membrane component is connected with first set Bipolar Membrane assembly salt room water-in, second water outlet and second overlaps Bipolar Membrane assembly salt room water-in and is connected, and the raffinate outlet of first, second cover Bipolar Membrane assembly is connected with a concentrating unit respectively.
4. system as claimed in claim 3, it is characterized in that, described concentrating unit comprises electrodialysis and reverse osmosis;
Preferably, described concentrating unit is set to one or both in electrodialysis or reverse osmosis.
5. system as claimed in claim 4, is characterized in that, the alkali room water outlet of first, second cover Bipolar Membrane assembly described all returns PH equalizing tank as regulating agent, and HF solution and H are reclaimed in the water outlet of sour room respectively 2sO 4solution.
6., as the system as described in arbitrary in claim 3-5, it is characterized in that, the dense water out of described concentrating unit all returns and is connected with the salt room water-in of its front end Bipolar Membrane assembly, dense water as the water inlet of salt room, fresh water discharge or recycle.
7. a separation method as claimed in claim 1, is characterized in that, described HF and H 2sO 4in mixing acid, HF content is 0.5% ~ 50%, H 2sO 4content is 0.5% ~ 98%.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110092355A (en) * 2019-06-06 2019-08-06 盛隆资源再生（无锡）有限公司 A method of hydrofluoric acid and ammonium salt are prepared using fluorine-containing nitrogen-containing wastewater

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2343256A1 (en) * 1973-08-28 1975-03-06 Wolfgang Dipl Chem Dr Konter PROCESS AND DEVICE FOR RECOVERING SULFURIC AND HYDROFLUORIC ACID FROM AN ACID MIXTURE IN PARTICULAR FROM THE POLISHING ACID IN THE ACID POLISHING PROCESS OF GRINDED GLASSES
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
CN103663547A (en) * 2012-09-24 2014-03-26 上海凯鑫分离技术有限公司 Treatment and recovery process of acid wastewater in titanium dioxide production process
CN103936214A (en) * 2013-08-02 2014-07-23 浙江赛特膜技术有限公司 Method for bipolar membrane electrodialysis treatment of 3-aminopyrazole-4-carboxamide hemisulfate production wastewater and recycling of sulfuric acid

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2343256A1 (en) * 1973-08-28 1975-03-06 Wolfgang Dipl Chem Dr Konter PROCESS AND DEVICE FOR RECOVERING SULFURIC AND HYDROFLUORIC ACID FROM AN ACID MIXTURE IN PARTICULAR FROM THE POLISHING ACID IN THE ACID POLISHING PROCESS OF GRINDED GLASSES
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
CN103663547A (en) * 2012-09-24 2014-03-26 上海凯鑫分离技术有限公司 Treatment and recovery process of acid wastewater in titanium dioxide production process
CN103936214A (en) * 2013-08-02 2014-07-23 浙江赛特膜技术有限公司 Method for bipolar membrane electrodialysis treatment of 3-aminopyrazole-4-carboxamide hemisulfate production wastewater and recycling of sulfuric acid

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110092355A (en) * 2019-06-06 2019-08-06 盛隆资源再生（无锡）有限公司 A method of hydrofluoric acid and ammonium salt are prepared using fluorine-containing nitrogen-containing wastewater

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