CN109160655A - A kind of metallurgy salty scrap acid recovery processing technique - Google Patents
A kind of metallurgy salty scrap acid recovery processing technique Download PDFInfo
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- CN109160655A CN109160655A CN201810963254.1A CN201810963254A CN109160655A CN 109160655 A CN109160655 A CN 109160655A CN 201810963254 A CN201810963254 A CN 201810963254A CN 109160655 A CN109160655 A CN 109160655A
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- acid
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- 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
- C01B17/901—Recovery from spent acids containing metallic ions, e.g. hydrolysis acids, pickling acids
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/14—Sulfates
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/34—Treatment of water, waste water, or sewage with mechanical oscillations
- C02F1/36—Treatment of water, waste water, or sewage with mechanical oscillations ultrasonic vibrations
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F2001/007—Processes including a sedimentation step
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
Abstract
The present invention relates to water treatment field more particularly to a kind of metallurgical salty scrap acid recovery processing techniques.Including precipitating, low temperature crystallization, separation of solid and liquid, security personnel filtering, second level nanofiltration, sour water separating step, the present invention crystallizes coupling membrane separation technique by using cryogenic freezing, realizes the separation and recycling of high-quality acid and crystal salt in salty scrap acid.Crystal salt can meet industrial application, and high-quality acid can use direct reuse, or be concentrated, and realize that the production of high-quality acid reduces environmental pollution to realize the recycling of resource.
Description
Technical field
The present invention relates to water treatment field more particularly to a kind of metallurgical salty scrap acid recovery processing techniques.
Background technique
In industrial circles such as coal mine, troilite, coal washing, chemical industry, printing and dyeing, metallurgy, a large amount of acid waste waters are used and generated, are had
It is distributed feature extensive, that blowdown flow rate is big, significant proportion is occupied in industrial wastewater.
By taking titanium white production as an example, the titanium dioxide in China 95% is all made of Production By Sulfuric Acid Process, and 1 ton of titanium dioxide of every production will be arranged
8 ~ 10 tons of spent acid are put, while generating a large amount of exhaust gas, waste water, waste residue.Contain 15 ~ 25% sulfuric acid and 10 ~ 15% sulphur in spent acid
It is sour ferrous, simultaneously containing aluminum sulfate, magnesium sulfate etc..According to current China's titanium dioxide production capacity, the sector produces 20% or so sulfur waste per year
Up to more than 1,000 ten thousand tons of acid, if generation seriously affected to ecological environment without processing direct emission.
The processing of country's spent acid dilute for titanium white or the technology of recycling have:
1, liquid ammonia vaporization is passed through in mixed liquor by neutralisation treatment by the way that ferrous sulfate is added in spent acid, and ferrous sulfate can be made
Ammonium；By being neutralized with lime stone, different process conditions are controlled, the products such as GYPSUM RUBRUM, white gypsum can be respectively obtained.
2, copper sulphate, phosphate fertilizer, synthetic rutile, bodied ferric sulfate etc. are prepared using spent acid.
3, concentration, spent acid are concentrated by " Top's Suo-Ni Luo atomization " concentration, roasting regeneration, Bayer vacuum multi-stage,
Spray concentration etc. obtains the sulfuric acid of high concentration.
4, the salinity in spent acid is absorbed using extractant, realizes hydrochlorate separation by extraction.
Substantially there is the features such as process flow is long, Related product purity is low in these technologies.
Summary of the invention
In view of the deficiencies of the prior art, the invention proposes a kind of metallurgical salty scrap acid recovery processing technique, pass through freezing
Crystallization couples acidproof film separation system, realizes the separation and recycling of high-quality acid and crystal salt in salty scrap acid.Sulfuric acid can be formed
Ferrous and high-purity sulfuric acid product, for selling or being back to use in production technology.The technology of present invention solution above-mentioned technical problem
Scheme is.A kind of metallurgy salty scrap acid recovery processing technique, comprising the following steps:
It is precipitated Step 1: metallurgical salty scrap acid is entered sedimentation basin, makes the particulate matters such as suspended matter in metallurgical salty scrap acid
It precipitates, and collects supernatant.
Step 2: supernatant obtained by step 1 is entered crystallization kettle crystallization treatment, will be crystallized by crystallization kettle external cold source
Temperature control using ultrasonic device or/and adds crystal seed initiation promotion crystallization formation at 1 ~ 8 DEG C, obtains crystallization spent acid and mixes
Liquid, the ultrasonic device supersonic frequency 15/20/24kHz, ultrasonic power 1800/2000/2600W, ultrasonic wave emit duration
0.2s, ultrasonic wave transmission interval 5-10s；
Step 3: being separated by solid-liquid separation as solid-liquid separating equipment to crystallization spent acid mixed liquor obtained by step 2, crystal salt is obtained
With spent acid clear liquid, gained crystal salt is discharged by the discharge outlet of solid-liquid separating equipment and is collected, and solid-liquid separating equipment is between 0-10 DEG C
Work reaches the removal rate of 50-80% to total salinity in crystallization spent acid mixed liquor；
It is carried out Step 4: spent acid clear liquid obtained by step 3 is entered cartridge filter, cartridge filter uses fiber bundle filter
Or core type filter, 5-50 μm of filtering accuracy, filtered fluid is obtained, impurity content in filtered fluid is reduced, reaches into acid-resistant disintegration
The requirement of separation system.
Step 5: the filtered fluid that step 4 is obtained, which enters acidproof film separation system, carries out sour water separation, the acid-resistant disintegration
Separation system is second level nanofiltration film separation system, and 70 bar of nanofiltration membrane highest proof pressure, 80 DEG C of highest tolerable temperature, retention divides
Son amount is 180 Da, and 90% or more salinity rejection does not form concentration through the salinity of second level nanofiltration membrane and acid in the filtered fluid
Liquid is back in crystallization kettle described in step 2, forms the acid solution of high-purity in the filtered fluid through the acid of second level nanofiltration membrane,
For the acid solution salt content less than 0.1%, acid concentration is 5 ~ 25%,
It is carried out Step 6: high purity acid solution obtained by step 5 enters sour water separator by reducing molten boiling point under vacuum conditions
Acid, water separation, sour water separator work temperature control between 40-80 DEG C, and pressure, will be sour molten in -0.09 ~ -0.06 Mpa
Acid in liquid is concentrated to 50-80% and forms concentrated acid, and vapor, which is then discharged into after condenser is condensed, to be discharged or collect.
The present invention couples acidproof film separation system using freezing and crystallizing, realizes high-quality acid and crystal salt in salty scrap acid
Separation and recycling, process route is easy, energy consumption is lower.The ferrous sulfate and gelled acid of formation can be sold outside or reuse, creates economical
Benefit, not only realizes the reuse of resource, but also avoids ecological environmental pollution, has achieved the purpose that zero-emission, is suitble to promote
Using.
Specific embodiment
A kind of metallurgical salty scrap acid recovery processing technique of the present invention, comprising the following steps:
It is precipitated Step 1: metallurgical salty scrap acid is entered sedimentation basin, makes the particulate matters such as suspended matter in metallurgical salty scrap acid
It precipitates, and collects supernatant.
Step 2: supernatant obtained by step 1 is entered crystallization kettle crystallization treatment, will be crystallized by crystallization kettle external cold source
Temperature controls 1 ~ 8 DEG C, and is caused using ultrasonic device and crystallization is promoted to be formed, and obtains crystallization spent acid mixed liquor, the ultrasonic device
Supersonic frequency 15/20/24kHz, ultrasonic power 1800/2000/2600W, ultrasonic wave emit duration 0.2s, ultrasonic wave transmission interval
5-10s；
Step 3: being separated by solid-liquid separation as solid-liquid separating equipment to crystallization spent acid mixed liquor obtained by step 2, crystal salt is obtained
With spent acid clear liquid, gained crystal salt is discharged by the discharge outlet of solid-liquid separating equipment and is collected, and solid-liquid separating equipment is between 0-10 DEG C
Work reaches the removal rate of 50-80% to total salinity in crystallization spent acid mixed liquor；
It being carried out Step 4: spent acid clear liquid obtained by step 3 is entered cartridge filter, cartridge filter uses fiber bundle filter,
5 μm of filtering accuracy, filtered fluid is obtained, impurity content in filtered fluid is made to reach the requirement for entering acidproof film separation system.
Step 5: the filtered fluid that step 4 is obtained, which enters acidproof film separation system, carries out sour water separation, the acid-resistant disintegration
Separation system is second level nanofiltration film separation system, and nanofiltration membrane is purchased from membrane technology (Shanghai) Co., Ltd. A product difficult to understand, and nanofiltration membrane is most
High 70 bar of proof pressure, 80 DEG C of highest tolerable temperature, molecular cut off is 180 Da, 90% or more salinity rejection, the mistake
The salinity through the film of second level nanofiltration membrane and acid formation concentrate are not back in crystallization kettle described in step 2 in filtrate, the mistake
The acid solution of high-purity is formed in filtrate through the acid of second level nanofiltration membrane, less than 0.1%, acid concentration is the acid solution salt content
15 ~ 25%,
It is carried out Step 6: high purity acid solution obtained by step 5 enters sour water separator by reducing molten boiling point under vacuum conditions
Acid, water separation, the control of sour water separator work temperature exist40-80Between DEG C, pressure, will be sour molten in -0.09 ~ -0.06 Mpa
Acid in liquid is concentrated to 50-80% and forms concentrated acid, and vapor, which is then discharged into after condenser is condensed, to be discharged or collect.
Embodiment 1:
10 tons of titanium white production acid waste waters (sulfuric acid concentration 21%, sulfate concentration 9%), after sedimentation basin precipitates, suspended matter
Equal particulate matters precipitate.Supernatant enters crystallization kettle, and control crystallization kettle temperature is 4 DEG C, sets ultrasonic device in crystallization kettle
Supersonic frequency 24kHz, ultrasonic power 2600W, ultrasonic wave emit duration 0.2s, ultrasonic wave transmission interval 5s, cause crystallization and are formed
Crystallize spent acid mixed liquor.Crystallization spent acid mixed liquor enters solid-liquid separator and is separated, and 8 DEG C of temperature, obtains crystal salt, spent acid is clear
Liquid sulfate concentration is reduced to 4% or so, by cartridge filter, into second level nanofiltration film separation system, second level nanofiltration UF membrane
The nanofiltration membrane of system is purchased from membrane technology (Shanghai) Co., Ltd. A-3012 product difficult to understand, 70 bar of nanofiltration membrane highest proof pressure,
80 DEG C of highest tolerable temperature.Through detecting, the 70% of total inflow is accounted for through the acid solution of second level nanofiltration film separation system, ingredient is
Concentration is the sulfate of 20% sulfuric acid and content 0.1%, is not back to knot through 30% concentrate of second level nanofiltration film separation system
Brilliant kettle causes sulfate concentration in crystallization reactor to be promoted, promotes the generation of crystallization, as system is run, second level nanofiltration membrane
System flowback is stablized, and handles 10 tons of diluted acids and obtains 0.897 ton of crystal salt altogether.The sulfuric acid that second level nanofiltration film separation system generates continues
Into sour water separator, under 65 DEG C, the vacuum condition of -0.09Mpa, low-temperature evaporation crystallisation by cooling is carried out, final acquisition 70%
About 2.84 tons of the concentrated sulfuric acid, condensate liquid outlet.
Embodiment 2:
10 tons of titanium white production acid waste waters (sulfuric acid concentration 17%, sulfate concentration 7%), after sedimentation basin precipitates, suspended matter
Equal particulate matters precipitate.Supernatant enters crystallization kettle, and control crystallization kettle temperature is 4 DEG C, sets ultrasonic device in crystallization kettle
Supersonic frequency 15kHz, ultrasonic power 1800W, ultrasonic wave emit duration 0.2s, ultrasonic wave transmission interval 5s, cause crystallization and is formed
Crystallize spent acid mixed liquor.Crystallization spent acid mixed liquor enters solid-liquid separator and is separated, and 8 DEG C of temperature, obtains crystal salt, spent acid is clear
Liquid sulfate concentration is reduced to 4% or so, by cartridge filter, into second level nanofiltration film separation system, second level nanofiltration UF membrane
The nanofiltration membrane of system is purchased from membrane technology (Shanghai) Co., Ltd. A series of products difficult to understand, and 70 bar of nanofiltration membrane proof pressure is arranged, resistance to
By 80 DEG C of temperature.Through detecting, the acid solution composition through second level nanofiltration film separation system is that concentration is 16% sulfuric acid and content 0.1%
Sulfate, be not back to crystallization kettle through 27% concentrate of second level nanofiltration film separation system, cause sulphur in crystallization reactor
Hydrochlorate concentration is promoted, and promotes the generation of crystallization, and as system is run, the reflux of second level nanofiltration membrane system is stablized, and 10 tons of processing is dilute
Acid obtains 0.696 ton of crystal salt altogether.The sulfuric acid that nanofiltration film separation system generates goes successively to sour water separator, at 58 DEG C ,-
Under the vacuum condition of 0.09Mpa, low-temperature evaporation crystallisation by cooling is carried out, about 2.3 tons of the concentrated sulfuric acid of 50% are finally obtained, outside condensate liquid
Row.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (1)
1. a kind of metallurgy salty scrap acid recovery processing technique, it is characterised in that: the following steps are included:
It is precipitated Step 1: metallurgical salty scrap acid is entered sedimentation basin, makes the particulate matters such as suspended matter in metallurgical salty scrap acid
It precipitates, and collects supernatant,
Step 2: supernatant obtained by step 1 is entered crystallization kettle crystallization treatment, by crystallization kettle external cold source by crystallization temperature
1-8 DEG C of control, and use ultrasonic device or/and add crystal seed initiation and crystallization is promoted to be formed, it obtains crystallizing spent acid mixed liquor, it is described
Ultrasonic device supersonic frequency 15/20/24kHz, ultrasonic power 1800/2000/2600W, ultrasonic wave transmitting duration 0.2s, ultrasonic wave
Transmission interval 5-10s；
Step 3: being separated by solid-liquid separation as solid-liquid separating equipment to crystallization spent acid mixed liquor obtained by step 2, crystal salt is obtained
With spent acid clear liquid, gained crystal salt is discharged by the discharge outlet of solid-liquid separating equipment and is collected, and solid-liquid separating equipment is between 0-10 DEG C
Work reaches the removal rate of 50-80% to total salinity in crystallization spent acid mixed liquor；
It is carried out Step 4: spent acid clear liquid obtained by step 3 is entered cartridge filter, cartridge filter uses fiber bundle filter
Or core type filter, 5-50 μm of filtering accuracy, filtered fluid is obtained, impurity content in filtered fluid is reduced, reaches into acid-resistant disintegration
The requirement of separation system,
Step 5: the filtered fluid that step 4 is obtained, which enters acidproof film separation system, carries out sour water separation, the acidproof UF membrane
System is second level nanofiltration film separation system, nanofiltration membrane highest proof pressure 70 bar, 80 DEG C of highest tolerable temperature, molecular cut off
For 180 Da, 90% or more salinity rejection does not form concentrate through the salinity of second level nanofiltration membrane and acid in the filtered fluid and returns
It flow in crystallization kettle described in step 2, forms the acid solution of high-purity in the filtered fluid through the acid of second level nanofiltration membrane, it is described
For acid solution salt content less than 0.1%, acid concentration is 5 ~ 25%,
It is carried out Step 6: high purity acid solution obtained by step 5 enters sour water separator by reducing molten boiling point under vacuum conditions
Acid, water separation, sour water separator work temperature control between 40-80 DEG C, and pressure, will be sour molten in-0.09-- 0.06 Mpa
Acid in liquid is concentrated to 50%-80% and forms concentrated acid, and vapor, which is then discharged into after condenser is condensed, to be discharged or collect.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110002510A (en) * | 2019-03-22 | 2019-07-12 | 烟台金正环保科技有限公司 | A kind of integrated technique of steel pickling waste liquor processing |
| CN110386720A (en) * | 2019-06-25 | 2019-10-29 | 广州安赛化工有限公司 | A kind of purifying of plating high-salt wastewater and salt separation system and treatment process |
| CN112159015A (en) * | 2020-09-09 | 2021-01-01 | 湖南恒晟环保科技有限公司 | Novel membrane separation and low-temperature evaporation concentration processing technology for waste acid |
| CN115340234A (en) * | 2021-05-13 | 2022-11-15 | 国家能源投资集团有限责任公司 | Wastewater treatment method, treatment system and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110002510A (en) * | 2019-03-22 | 2019-07-12 | 烟台金正环保科技有限公司 | A kind of integrated technique of steel pickling waste liquor processing |
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