CN110668401B - Harmless disposal and resource utilization method of high-salt waste acid - Google Patents
Harmless disposal and resource utilization method of high-salt waste acid Download PDFInfo
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- CN110668401B CN110668401B CN201910783830.9A CN201910783830A CN110668401B CN 110668401 B CN110668401 B CN 110668401B CN 201910783830 A CN201910783830 A CN 201910783830A CN 110668401 B CN110668401 B CN 110668401B
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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
- C01B7/195—Separation; Purification
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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
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/88—Concentration of sulfuric acid
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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
- 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
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
- C01B21/38—Nitric acid
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
- C01B21/50—Nitrous acid; Salts thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
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- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/02—Preparation of sulfates from alkali metal salts and sulfuric acid or bisulfates; Preparation of bisulfates
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Abstract
A harmless disposal and resource utilization method of high-salt waste acid comprises the steps of firstly controlling process conditions to sequentially remove hydrogen fluoride and dichloromethane in the high-salt waste acid, absorbing the hydrogen fluoride with water to obtain hydrofluoric acid, and condensing dichloromethane gas to obtain dichloromethane; cooling, crystallizing and separating the waste acid after separating hydrogen fluoride and dichloromethane to obtain crude potassium bisulfate and waste acid I, adding a decomposing agent into the waste acid I to decompose sulfamic acid contained in the waste acid I to generate potassium bisulfate and nitrogen, obtaining waste acid II after decomposing sulfamic acid, crystallizing and separating the waste acid II at low temperature to obtain crude potassium bisulfate and neutral acid, and evaporating to obtain industrial sulfuric acid with the concentration of not less than 90%. And (3) treating the crude potassium bisulfate by adopting a recrystallization method to obtain the industrial potassium bisulfate. The effective separation of acid and salt and the effective removal of other organic and inorganic impurities in the high-salt waste acid are realized. The obtained product is potassium bisulfate/potassium sulfate and industrial sulfuric acid which meet the industrial requirements, and realizes resource utilization of waste acid while performing harmless treatment.
Description
Technical Field
The invention belongs to the technical field of wastewater treatment, and particularly relates to a method for harmless treatment and resource utilization of high-salinity waste acid.
Background
The high-salt waste acid is electrolyte required by new energy industry, such as waste sulfuric acid generated in the production process of lithium bis (fluorosulfonyl) imide and the like, and mainly comprises the following chemical components: sulfuric acid, potassium bisulfate, potassium sulfate, dichloromethane, hydrogen fluoride and sulfamic acid. Wherein sulfuric acid and potassium bisulfate are taken as main components. Because the high-salt waste acid has complex components and is difficult to harmlessly treat and recycle, no good treatment method exists at present, and no report on harmlessness treatment and recycling of the high-salt waste acid exists.
Disclosure of Invention
In order to solve the problems of harmless treatment and resource utilization of the high-salt waste acid, the invention discloses a harmless treatment and resource utilization method of the high-salt waste acid.
1, a harmless treatment and resource utilization method of high-salt waste acid, which is characterized by comprising the following steps:
the method comprises the following steps: and (3) sequentially removing hydrogen fluoride and dichloromethane in the high-salt waste acid by adopting a separation device, absorbing the hydrogen fluoride by using water to obtain hydrofluoric acid, condensing dichloromethane gas to obtain dichloromethane, or collecting the hydrogen fluoride and the dichloromethane gas and conveying the collected gas to other related procedures for centralized disposal or utilization.
And step two, cooling, crystallizing and separating the waste acid after separating the hydrogen fluoride and the dichloromethane under the condition of negative pressure or no contact with air to obtain crude potassium bisulfate and waste acid I.
Step three: and adding a decomposing agent into the waste acid I to decompose the contained sulfamic acid to generate potassium bisulfate and nitrogen, and discharging the nitrogen harmlessly to obtain waste acid after decomposition of the sulfamic acid, namely waste acid II. And tail gas generated in the decomposition process is absorbed by alkali liquor or water to obtain absorption liquid, and the absorption liquid is returned to the decomposition process for recycling.
Step four: crystallizing and separating the waste acid II at low temperature to obtain crude potassium bisulfate and medium acid with the concentration of 60-75%, and evaporating the medium acid water to obtain industrial sulfuric acid with the concentration of not less than 93%.
Step five: and (3) treating the crude potassium bisulfate obtained in the second step and the fourth step by adopting a recrystallization method to obtain industrial potassium bisulfate, or directly reacting the crude potassium bisulfate with any one or more of potassium chloride/potassium hydroxide/potassium carbonate to produce potassium sulfate.
Preferably, the separation device in the step one is a tank reactor with a heating and stirring device, or a spray dissociation tower, and the treatment process is carried out under the condition of negative pressure or without contact with air.
Preferably, in the third step, a decomposing agent is added for removing sulfamic acid in the waste acid II, wherein the decomposing agent is one or more of nitrous acid and salts thereof, and the treatment process is carried out under the condition of negative pressure or without contact with air.
Preferably, side reactions occur in the decomposition process of the sulfamic acid in the third step to generate nitric oxide and nitrogen dioxide, the tail gas is treated by adopting an alkali absorption or water absorption mode, and the obtained nitrous acid or nitrite solution is returned to the decomposition process in the third step to be circularly used as a decomposing agent.
Preferably, in the third step, the nitrogen monoxide and nitrogen dioxide gas generated by the side reaction in the decomposition process of sulfamic acid is treated by a mode of absorbing with alkali or water, wherein the alkali is one or more of potassium hydroxide, potassium carbonate and sodium hydroxide.
Preferably, in the fifth step, the coarse potassium bisulfate is treated by a recrystallization method to obtain industrial potassium bisulfate, the used solvent is water, when the solvent is recycled until the concentration of sulfuric acid reaches more than 60%, the solvent is sent to the third step to be mixed with waste acid II for low-temperature crystallization, after the potassium bisulfate is separated out, the coarse potassium bisulfate and the neutral acid are separated and collected, further, the moisture in the neutral acid is evaporated to obtain more than 93% of industrial sulfuric acid, or the neutral potassium bisulfate is sent to the second step to be mixed with the waste acid I, and the mixture enters a subsequent related disposal process.
Preferably, the crystallization in the second step is carried out under the condition of negative pressure or no contact with air, and the crystallization temperature is 25-35 ℃.
Preferably, the low-temperature crystallization in the fourth step is carried out under the condition of negative pressure or no contact with air, the crystallization temperature is-20-10 ℃, and the crystallization time is 2-24 hours.
Preferably, in the step five, when the obtained crude potassium bisulfate is directly used for producing potassium sulfate, the crude potassium bisulfate is dissolved by water or circulating mother liquor, potassium hydroxide or potassium carbonate is used for neutralizing to generate potassium sulfate, then the potassium sulfate and the potassium sulfate mother liquor are obtained by separation, and the mother liquor is returned to the crude potassium bisulfate dissolving procedure for recycling.
Adopt above-mentioned technical scheme's advantage:
1. the effective separation of acid and salt and the effective removal of other organic and inorganic impurities in the high-salt waste acid are realized.
2. The treatment process does not generate wastewater and waste residues, the generated waste gas is effectively controlled, and the whole production process is environment-friendly and harmless.
3. The obtained products are potassium bisulfate/potassium sulfate and industrial sulfuric acid which meet industrial requirements, and the resource utilization of the waste acid is realized while harmless treatment is carried out.
4. The process of the invention is used for harmless treatment and resource utilization of the high-salt waste acid, eliminates the environmental burden of electrolyte production enterprises required by new energy industries due to the generation of the high-salt waste acid, has low treatment cost, meets the market demand of products, and has good environmental benefit and economic benefit.
Detailed Description
Example 1:
the processed materials are high-salt waste acid generated by electrolyte production enterprises required by new energy industries, and the components are as follows: h2SO456.94%，KHSO438.57%，HF1.56%，CH2Cl21.64 percent and 1.29 percent of sulfamic acid.
The harmless treatment and resource utilization method of the high-salt waste acid comprises the following steps:
the method comprises the following steps: the method comprises the following steps of sequentially removing hydrogen fluoride and dichloromethane in high-salt waste acid by adopting a kettle type reactor with a heating and stirring device or a spray dissociation tower under the condition of negative pressure or no contact with air, absorbing the hydrogen fluoride by using water to obtain hydrofluoric acid, condensing dichloromethane gas to obtain dichloromethane, or collecting the hydrogen fluoride and the dichloromethane gas and sending the collected gas to other related procedures for centralized disposal or utilization.
And step two, cooling, crystallizing and separating the waste acid after separating the hydrogen fluoride and the dichloromethane under the condition of negative pressure or no contact with air to obtain crude potassium bisulfate and waste acid I, wherein the crystallization is carried out under the condition of negative pressure or no contact with air, and the crystallization temperature is 25-35 ℃.
Step three: adding a decomposer into the waste acid I to decompose the contained sulfamic acid to generate potassium bisulfate and nitrogen, wherein the decomposer is one or more of potassium nitrite, sodium nitrite, nitrous acid and salts thereof, and the treatment process is carried out under the condition of negative pressure or no contact with air; and (4) harmlessly exhausting nitrogen, and decomposing to obtain waste acid after decomposing sulfamic acid, namely waste acid II. And tail gas generated in the decomposition process is absorbed by alkali liquor or water to obtain absorption liquid, and the absorption liquid is returned to the decomposition process for recycling. The alkali is one or more of potassium hydroxide, potassium carbonate and sodium hydroxide, and potassium hydroxide is preferred.
Step four: and crystallizing and separating the waste acid II at low temperature to obtain crude potassium bisulfate and neutral acid with the concentration of 60-75%, evaporating the neutral acid water to obtain industrial sulfuric acid with the concentration of not less than 93%, wherein the low-temperature crystallization is carried out under the conditions of negative pressure or no contact with air, the crystallization temperature is-20-10 ℃, and the crystallization time is 2-24 hours. .
Step five: and (3) treating the crude potassium bisulfate obtained in the second step and the fourth step by adopting a recrystallization method to obtain industrial potassium bisulfate, wherein the used solvent is water, when the solvent is recycled until the concentration of sulfuric acid reaches more than 60%, the solvent is sent to the third step to be mixed with waste acid II for low-temperature crystallization, after the potassium bisulfate is separated out, the crude potassium bisulfate and neutral acid are separated and collected, further, the moisture in the neutral acid is evaporated to obtain the industrial sulfuric acid with the concentration of more than 93%, or the crude potassium bisulfate is sent to the second step to be mixed with the waste acid I, and the industrial potassium bisulfate enters a subsequent related treatment process.
Or dissolving the crude potassium bisulfate in water or circulating mother liquor, directly reacting with any one or more of potassium chloride/potassium hydroxide/potassium carbonate to produce potassium sulfate, and then separating to obtain the potassium sulfate and the potassium sulfate mother liquor. And returning the mother liquor to the crude potassium bisulfate dissolving process for recycling.
According to the harmless treatment and resource utilization method of the high-salt waste acid, 1000kg of the high-salt waste acid is put into a production system for treatment, the yield of HF is 93.06 percent, and CH is recovered2Cl2The yield was 95.87%, the decomposition rate of sulfamic acid was 95.41%, the crystallization rate of potassium bisulfate was 99.31%, the yield of sulfuric acid was 99.30%, and the yield of potassium bisulfate was 99.82%.
The sulfuric acid is obtained by treatment, the content is 93.61 percent, and the standard GB/T534-2014 is met; 415kg of potassium bisulfate with the content of 96.43 percent is obtained, which meets the industrial requirements; 46.5kg of hydrogen fluoride solution with the content of 31.22 percent is obtained, and the standard of GB 7744-; 15.8kg of dichloromethane is obtained, the content is 99.51 percent, and the GB/T4117-2008 standard is met.
Example 2:
the processed materials are high-salt waste acid generated by electrolyte production enterprises required by new energy industries, and the components are as follows: h2SO448.58%，KHSO443.62%，HF2.63%，CH2Cl22.41 percent and 2.76 percent of sulfamic acid.
According to the harmless treatment and resource utilization method of the high-salt waste acid, 1000kg of high-salt waste acid is put into a production system for treatment, the yield of HF is 92.97%, and CH is recovered2Cl2The yield was 94.41%, the decomposition rate of sulfamic acid was 96.27%, and sulfur was containedThe crystallization rate of the potassium hydrogen sulfate is 99.82 percent, the yield of the sulfuric acid is 99.86 percent, and the yield of the potassium sulfate is 99.24 percent.
390kg of sulfuric acid is obtained through treatment, the content is 92.78 percent, and the standard of GB/T534-2014 is met; 842kg of potassium sulfate is obtained, the content of potassium oxide is 52.37 percent, and the standard of GB/T20406-2017 is met; 79.0kg of hydrogen fluoride solution with the content of 30.95 percent is obtained, and the standard of GB 7744-; 22.9kg of dichloromethane is obtained, the content is 99.36 percent, and the standard GB/T4117-2008 is met.
Claims (9)
1. A harmless treatment and resource utilization method of high-salt waste acid is characterized by comprising the following steps:
the method comprises the following steps: sequentially removing hydrogen fluoride and dichloromethane in the high-salt waste acid by adopting separation equipment, absorbing the hydrogen fluoride by using water to obtain hydrofluoric acid, and condensing dichloromethane gas to obtain dichloromethane; or collecting the hydrogen fluoride and the dichloromethane gas and sending the hydrogen fluoride and the dichloromethane gas to other related procedures for centralized disposal or utilization;
step two, cooling, crystallizing and separating the waste acid after separating the hydrogen fluoride and the dichloromethane under the condition of negative pressure or no contact with air to obtain crude potassium bisulfate and waste acid
；
Step three: adding a decomposing agent into the waste acid I to decompose the sulfamic acid to generate potassium bisulfate and nitrogen, and discharging the nitrogen harmlessly to obtain the waste acid after decomposition of the sulfamic acid, namely the waste acid
(ii) a Absorbing tail gas generated in the decomposition process by using alkali liquor or water to obtain absorption liquid, and returning the absorption liquid to the decomposition process for recycling;
step four: crystallizing and separating the waste acid II at low temperature to obtain crude potassium bisulfate and neutral acid with the concentration of 60-75%, and evaporating the neutral acid water to obtain industrial sulfuric acid with the concentration of not less than 93%;
step five: and (3) treating the crude potassium bisulfate obtained in the second step and the fourth step by adopting a recrystallization method to obtain industrial potassium bisulfate, or directly reacting the crude potassium bisulfate with any one or more of potassium chloride/potassium hydroxide/potassium carbonate to produce potassium sulfate.
2. The harmless disposal and resource utilization method of high-salinity waste acid according to claim 1, characterized in that: the separation equipment in the step one is a kettle type reactor with a heating and stirring device or a spray type dissociation tower, and the treatment process is carried out under the condition of negative pressure or no contact with air.
3. The harmless disposal and resource utilization method of high-salinity waste acid according to claim 1, characterized in that: in the third step, the decomposing agent is one or more of nitrous acid and salts thereof, and the treatment process is carried out under the condition of negative pressure or without contact with air.
4. The harmless disposal and resource utilization method of high-salinity waste acid according to claim 1, characterized in that: thirdly, side reactions occur in the decomposition process of the sulfamic acid to generate nitric oxide and nitrogen dioxide; and the tail gas treatment method adopts an alkali absorption or water absorption mode to treat, and the obtained nitrous acid or nitrite solution is returned to the decomposition working procedure in the third step to be circularly used as a decomposing agent.
5. The harmless disposal and resource utilization method of high-salinity waste acid according to claim 1, characterized in that: and step three, treating nitrogen monoxide and nitrogen dioxide gas generated by side reaction in the decomposition process of sulfamic acid in a mode of absorbing by alkali or water, wherein the alkali is one or more of potassium hydroxide, potassium carbonate and sodium hydroxide.
6. The harmless disposal and resource utilization method of high-salinity waste acid according to claim 1, characterized in that: step five, treating the crude potassium bisulfate by adopting a recrystallization method to obtain industrial potassium bisulfate, wherein the used solvent is water, when the solvent is recycled until the concentration of sulfuric acid reaches more than 60 percent, the solvent is sent to the step three to be mixed with waste acid II for low-temperature crystallization, after the potassium bisulfate is separated out, the crude potassium bisulfate and the neutral acid are separated and obtained, and further, the moisture in the neutral acid is evaporated to obtain the industrial sulfuric acid with the concentration of more than 93 percent; or the mixture is sent to the step two to be mixed with the waste acid I and enters a subsequent relevant disposal procedure.
7. The harmless disposal and resource utilization method of high-salinity waste acid according to claim 1, characterized in that: and the crystallization in the second step is carried out under the condition of negative pressure or no contact with air, and the crystallization temperature is 25-35 ℃.
8. The harmless disposal and resource utilization method of high-salinity waste acid according to claim 1, characterized in that: and the low-temperature crystallization in the step four is carried out under the condition of negative pressure or no contact with air, the crystallization temperature is-20-10 ℃, and the crystallization time is 2-24 hours.
9. The harmless disposal and resource utilization method of high-salinity waste acid according to claim 1, characterized in that: and fifthly, when the obtained crude potassium bisulfate is directly used for producing potassium sulfate, dissolving the crude potassium bisulfate by using water or circulating mother liquor, neutralizing by using potassium hydroxide or potassium carbonate to generate the potassium sulfate, separating to obtain the potassium sulfate and the potassium sulfate mother liquor, and returning the mother liquor to the crude potassium bisulfate dissolving procedure for recycling.
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| CN111520975A (en) * | 2020-06-02 | 2020-08-11 | 湖南省湘衡盐化有限责任公司 | Industrial salt drying system and method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2134270C (en) * | 1994-10-25 | 2005-07-26 | Drew John Drexler | Nox destruction in sulphuric acid |
| CN104386654A (en) * | 2014-11-17 | 2015-03-04 | 云南华联锌铟股份有限公司 | Method for treating acidic wastewater of sulfide ore roasted flue gas acid manufacture system |
| CN109574388A (en) * | 2018-12-13 | 2019-04-05 | 佛山市碧沃丰生物科技股份有限公司 | A kind of minimizing technology of high concentration sulfamate waste water total nitrogen |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2134270C (en) * | 1994-10-25 | 2005-07-26 | Drew John Drexler | Nox destruction in sulphuric acid |
| CN104386654A (en) * | 2014-11-17 | 2015-03-04 | 云南华联锌铟股份有限公司 | Method for treating acidic wastewater of sulfide ore roasted flue gas acid manufacture system |
| CN109574388A (en) * | 2018-12-13 | 2019-04-05 | 佛山市碧沃丰生物科技股份有限公司 | A kind of minimizing technology of high concentration sulfamate waste water total nitrogen |
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