CN102863036A - Method for regeneration of hydrochloric acid containing waste liquid by means of microwave heating - Google Patents
Method for regeneration of hydrochloric acid containing waste liquid by means of microwave heating Download PDFInfo
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- CN102863036A CN102863036A CN2012103561899A CN201210356189A CN102863036A CN 102863036 A CN102863036 A CN 102863036A CN 2012103561899 A CN2012103561899 A CN 2012103561899A CN 201210356189 A CN201210356189 A CN 201210356189A CN 102863036 A CN102863036 A CN 102863036A
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- Prior art keywords
- microwave heating
- waste liquid
- hydrochloric
- hydrochloric acid
- acid
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000010438 heat treatment Methods 0.000 title claims abstract description 30
- 239000007788 liquid Substances 0.000 title claims abstract description 24
- 239000002699 waste material Substances 0.000 title claims abstract description 21
- 230000008929 regeneration Effects 0.000 title claims abstract description 10
- 238000011069 regeneration method Methods 0.000 title claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 12
- 238000009835 boiling Methods 0.000 claims description 13
- 238000009833 condensation Methods 0.000 claims description 7
- 230000005494 condensation Effects 0.000 claims description 7
- 230000001172 regenerating effect Effects 0.000 claims description 7
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 5
- 229910001424 calcium ion Inorganic materials 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 18
- 238000011084 recovery Methods 0.000 abstract description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 abstract description 4
- 238000004064 recycling Methods 0.000 abstract description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 2
- 230000018109 developmental process Effects 0.000 abstract description 2
- 239000003814 drug Substances 0.000 abstract description 2
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 2
- 238000003889 chemical engineering Methods 0.000 abstract 1
- 235000011167 hydrochloric acid Nutrition 0.000 description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- 238000001704 evaporation Methods 0.000 description 5
- 230000008020 evaporation Effects 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000012528 membrane Substances 0.000 description 3
- 238000007599 discharging Methods 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000502 dialysis Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000007131 hydrochloric acid regeneration reaction Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000003014 ion exchange membrane Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 238000001471 micro-filtration Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
Abstract
The invention provides a method for regeneration of hydrochloric acid containing waste liquid by means of microwave heating. The method includes: subjecting the hydrochloric acid containing waste liquid to microwave heating until the liquid is boiled under the negative pressure of 0.08Mpa, and generated steam is condensed and collected to obtain regenerated hydrochloric acid. Acid recovery is thorough, and chloride ion content in residue liquid is lower than 0.2%; production devices are less, occupied area is small, heat exchange procedures are less, and energy utilization rate and heating efficiency are high; and safety, environment protection, cleaner production and zero pollution are realized, production cost is greatly reduced, operating efficiency is improved, and effective comprehensive utilization of resources is realized. The method can be widely applied to the production process of recycling of valuable acid recovered from waste liquid containing hydrochloric acid, nitric acid or hydrofluoric acid in the industries of metallurgy, chemical engineering, medicament, electronics and the like, and is significant to energy conversation, emission reduction, cleaner production and scientific development of enterprises.
Description
Technical field
The present invention relates to a kind of method of microwave heating waste hydrochloric acid regeneration, belong to the micro-wave energy applied technical field.
Background technology
In some Metal smelting enterprise production process, unavoidably can produce a large amount of waste hydrochloric acids.If the valency acid recovery that has is wherein recycled the pollution that can effectively control environment, Cost reduction drops into, and realizes recycling economy.
For the manipulation of regeneration of hydrochloric waste liquid, mainly contain at present following several method both at home and abroad:
1, high-temperature roasting method: high-temperature roasting method is with spent acid solution roasting under the hot conditions about 800 ℃, on the one hand, hydrochloric acid and water in the spent acid are evaporated, on the other hand, wherein contained metal chloride reacts with oxygen under hot conditions, produces simultaneously HC1 gas.The high temperature HC1 gas of the hydrochloric acid vapour that evaporates in the burning process and water vapor and generation absorbs by water, can obtain concentration and be about 20% hydrochloric acid.This method treatment capacity is large, and HCl recovery is more thorough, but investment is large, and operating ambient temperature is high, working cost is high, requires level of management high, only is fit to large-scale enterprise and uses.
2, ion exchange method: ion exchange method is to utilize some example exchange resin can absorb acid from spent acid solution and the function of discharging metal-salt realizes a kind of method that acid separates with salt.But the advantage of this method is normal temperature to be processed, and energy consumption is low, and technical process is short, but the concentration of hydrochloric acid that reclaims is on the low side, and the rate of recovery is relatively poor, needs to add more concentrated hydrochloric acid in the production process and just can reuse.
3, membrane separation process: membrane separation process is to make spent acid enter the diffusion dialysis device, utilize the selection perviousness of ion-exchange membrane to make free acid constantly enter mutually water by spent acid, this method can make the rate of recovery of spent acid Free Acid reach more than 80%, to the rejection of metal-salt greater than 90%.Need to process through micro-filtration (≤5 μ m) but weak point is all stock liquids, maximum operation (service) temperature only is 40 ℃ in the process.The too high too early damage that causes ionic membrane of use temperature in the work-ing life of shortening film, needs the processing of lowering the temperature with the feed liquid of certain temperature in the operational process.So greatly affected production efficiency, be unfavorable for that the serialization of producing carries out.
4, heat steam heating method: mainly be to produce high-temperature vapor by coal firing boiler, utilize graphite heat exchanger with the heat transferred spent acid of high-temperature vapor, hydrochloric acid was reclaimed in evaporation after spent acid was heated to boiling.But in actual production, there are problems in above-mentioned heat transfer process: the graphite impact resistance in the graphite heat exchanger is lower, therefore when transportation, installation and operation, causes easily damage; More or less be dissolved with salts substances in the spent acid, be evaporated to a certain amount of later on meeting crystallization at spent acid, thereby in the process of circulation, stop up the graphite heat exchanger pipeline, and the cleaning difficulty is large, have a strong impact on production and carry out smoothly, can bring hidden danger to safety in production in addition; The high-temperature steam that boiler produces is after pipeline transmission, and to spent acid solution, after heat was transmitted so several times, heat utilization ratio was very low by the graphite heat exchanger heat exchange, causes the significant wastage of the too high and energy of production cost.
Summary of the invention
The technical problem to be solved in the present invention provides the method for the hydrochloric spent solution regeneration of a kind of microwave heating, the method can be carried out direct heating to hydrochloric waste liquid and be reclaimed hydrochloric acid, there is not heat transfer process, in addition, it is not high to have solved acid recovering rate, and operating ambient temperature is crossed the problems such as high, realizes safety in production, resource circulation utilization improves enterprise competitiveness.
The present invention realizes by following technical proposal: the method for the hydrochloric spent solution regeneration of a kind of microwave heating, process the following step: under the suction function of 0.05～0.08Mpa, by extremely boiling of microwave heating, the steam of generation is collected after condensation and is namely obtained the hydrochloric acid of regenerating with hydrochloric waste liquid.
During described employing microwave heating, the operating frequency of microwave is 2450MHz.
Described hydrochloric waste liquid refers to that chlorine ion concentration is the abraum salt acid solution of 60～140g/L.
Described hydrochloric waste liquid also contains sulfate ion and the sl. sol. calcium ion that concentration is 10～50g/L.
Under condition of negative pressure, microwave heating can make the temperature of spent acid solution raise rapidly quickly and effectively, thereby reaches boiling temperature, and this boiling temperature is than low 20 ℃ approximately of the boiling temperatures under the condition of normal pressure; Utilizing microwave heating principle, mainly is to utilize microwave to the effect of polar molecule, to the spent acid solution direct heating to boiling temperature and keep boiling state; Be conducive to like this produce energy-conservation; At hydrochloric waste liquid the phase transition process of gaseous state occurs to become from liquid state, steam is collected after condensation and is obtained the hydrochloric acid of regenerating.
The present invention adopts microwave heating, do not need heat transfer process, do not need thermal conduction from outward appearance to inner essence yet, but directly heat by the waste of energy of microwave at liquid internal, water and acid belong to polar molecule, and their specific inductivity is very high, belong to strong suction ripple material, microwave heating can make the temperature of spent acid solution raise rapidly timely and effectively, thereby reaches boiling temperature.
The present invention compared with prior art, its major advantage is: adopt microwave heating, rate of heating is fast, is easy to control, and is easy to operate; Acid recovery is comparatively thorough, and chloride ion content is lower than 0.2% in the raffinate; Without boiler and graphite heat exchanger, production unit is few, and floor space is few, does not have too much heat exchange link, and energy utilization rate and heating efficiency are high; Safety and environmental protection, cleaner production is pollution-free, greatly reduces production costs, and increases work efficiency, and forms effective comprehensive utilization of resources.That the present invention can be widely applied to is hydrochloric in the industries such as metallurgy, chemical industry, medicine and electronic industry, nitric acid or hydrofluoric acid waste liquid reclaim on the production technique that valency acid recycling is arranged, and industry energy conservation is reduced discharging, and cleaner production realizes that scientific development is significant.
Embodiment
The present invention will be further described below in conjunction with embodiment.
Embodiment 1
Under the suction function of 0.08Mpa, the hydrochloric waste liquid that with chlorine ion concentration is 60g/L by operating frequency be the microwave heating of 2450MHz to boiling, the steam of generation is collected after condensation and is namely obtained the hydrochloric acid of regenerating.The chlorine ion concentration that records behind the consecutive evaporation 5h in the raffinate only is 0.08%.
Embodiment 2
Under the suction function of 0.05Mpa, with chlorine ion concentration be 140g/L, sulfate ion and sl. sol. calcium ion concn be 10g/L hydrochloric waste liquid by operating frequency be 2450MHz microwave heating to the boiling, the steam of generation is collected after condensation and is namely obtained the hydrochloric acid of regenerating.The chlorine ion concentration that records behind the consecutive evaporation 4.5h in the raffinate only is 0.12%.
Embodiment 3
Under the suction function of 0.06Mpa, with chlorine ion concentration be 100g/L, sulfate ion and sl. sol. calcium ion concn be 40g/L hydrochloric waste liquid by operating frequency be 2450MHz microwave heating to the boiling, the steam of generation is collected after condensation and is namely obtained the hydrochloric acid of regenerating.The chlorine ion concentration that records behind the consecutive evaporation 4h in the raffinate only is 0.10%.
Embodiment 4
Under the suction function of 0.08Mpa, with chlorine ion concentration be 120g/L, sulfate ion and sl. sol. calcium ion concn be 50g/L hydrochloric waste liquid by operating frequency be 2450MHz microwave heating to the boiling, the steam of generation is collected after condensation and is namely obtained the hydrochloric acid of regenerating.The chlorine ion concentration that records behind the consecutive evaporation 5h in the raffinate only is 0.09%.
Claims (4)
1. the method for the hydrochloric spent solution regeneration of microwave heating is characterized in that through the following step: under the suction function of 0.05～0.08Mpa, with hydrochloric waste liquid by microwave heating to boiling, the steam of generation is collected after condensation and is namely obtained the hydrochloric acid of regenerating.
2. the method for the hydrochloric spent solution regeneration of microwave heating according to claim 1, it is characterized in that: during described employing microwave heating, the operating frequency of microwave is 2450MHz.
3. the method for the hydrochloric spent solution regeneration of microwave heating according to claim 1 and 2, it is characterized in that: described hydrochloric waste liquid refers to that chlorine ion concentration is the abraum salt acid solution of 60～140g/L.
4. the method for the hydrochloric spent solution regeneration of microwave heating according to claim 3, it is characterized in that: described hydrochloric waste liquid also contains sulfate ion and the sl. sol. calcium ion that concentration is 10～50g/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103561899A CN102863036A (en) | 2012-09-24 | 2012-09-24 | Method for regeneration of hydrochloric acid containing waste liquid by means of microwave heating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103561899A CN102863036A (en) | 2012-09-24 | 2012-09-24 | Method for regeneration of hydrochloric acid containing waste liquid by means of microwave heating |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102863036A true CN102863036A (en) | 2013-01-09 |
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| CN2012103561899A Pending CN102863036A (en) | 2012-09-24 | 2012-09-24 | Method for regeneration of hydrochloric acid containing waste liquid by means of microwave heating |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271429A (en) * | 2015-10-27 | 2016-01-27 | 昆明理工大学 | Method for preparing iron oxide red and hydrochloric acid from hot galvanized waste acid |
| CN115571893A (en) * | 2022-05-11 | 2023-01-06 | 陕西华特新材料股份有限公司 | Method for extracting and recovering boric acid from low-concentration hydrochloric acid waste liquid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1511058A (en) * | 2000-12-15 | 2004-07-07 | 普莱克斯技术有限公司 | Method of vaporizing liquids by microwave heating |
| CN101435082A (en) * | 2008-12-05 | 2009-05-20 | 同济大学 | Method for processing pickle liquor by negative pressure outer circulation continuous evaporation continuous freezing crystallization process |
| CN102774908A (en) * | 2012-08-21 | 2012-11-14 | 昆明理工大学 | Method for regenerating hydrochloric acid by microwave heating hydrochloric acid-containing waste liquid |
-
2012
- 2012-09-24 CN CN2012103561899A patent/CN102863036A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1511058A (en) * | 2000-12-15 | 2004-07-07 | 普莱克斯技术有限公司 | Method of vaporizing liquids by microwave heating |
| CN101435082A (en) * | 2008-12-05 | 2009-05-20 | 同济大学 | Method for processing pickle liquor by negative pressure outer circulation continuous evaporation continuous freezing crystallization process |
| CN102774908A (en) * | 2012-08-21 | 2012-11-14 | 昆明理工大学 | Method for regenerating hydrochloric acid by microwave heating hydrochloric acid-containing waste liquid |
Non-Patent Citations (1)
| Title |
|---|
| 赵俊学等: "不锈钢酸洗废水的微波加热蒸酸试验研究", 《湿法冶金》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271429A (en) * | 2015-10-27 | 2016-01-27 | 昆明理工大学 | Method for preparing iron oxide red and hydrochloric acid from hot galvanized waste acid |
| CN115571893A (en) * | 2022-05-11 | 2023-01-06 | 陕西华特新材料股份有限公司 | Method for extracting and recovering boric acid from low-concentration hydrochloric acid waste liquid |
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| PB01 | Publication | ||
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Application publication date: 20130109 |