CN115124179A - Treatment process of waste sulfuric acid - Google Patents
Treatment process of waste sulfuric acid Download PDFInfo
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- CN115124179A CN115124179A CN202210906174.9A CN202210906174A CN115124179A CN 115124179 A CN115124179 A CN 115124179A CN 202210906174 A CN202210906174 A CN 202210906174A CN 115124179 A CN115124179 A CN 115124179A
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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
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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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
- 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
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/26—Treatment of water, waste water, or sewage by extraction
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/76—Treatment of water, waste water, or sewage by oxidation with halogens or compounds of halogens
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention discloses a treatment process of waste sulfuric acid, and relates to the field of chemical industry. The treatment process of the waste sulfuric acid comprises the following steps: primary filtering, cooling and extracting, secondary filtering, tertiary filtering and high-temperature concentrating; firstly, carrying out filter pressing on the waste sulfuric acid to remove solid impurities, and obtaining primary filtered waste sulfuric acid; cooling and extracting the waste sulfuric acid subjected to primary filtration to remove quinoline to obtain cooled and extracted waste sulfuric acid; then adding zinc hydroxide into the cooled and extracted waste sulfuric acid, and performing filter pressing to obtain secondarily filtered waste sulfuric acid; then introducing chlorine into the waste sulfuric acid subjected to secondary filtration for filtration to obtain waste sulfuric acid subjected to tertiary filtration and filter residue zinc chloride pyridine complex salt, carrying out alkali decomposition on the zinc chloride pyridine complex salt to obtain zinc hydroxide, and putting the zinc hydroxide into secondary filtration for use again; and finally, concentrating the waste sulfuric acid filtered for three times at high temperature to obtain treated sulfuric acid, and spraying the tail gas by using hot alkali liquor. The treatment process of the waste sulfuric acid has the advantages of simple process steps, environmental protection, low energy consumption, high concentration of the treated sulfuric acid and low COD value.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a treatment process of waste sulfuric acid.
Background
The waste sulfuric acid from refining crude benzene is the waste liquid produced in the acid washing process of benzene production in coking plant. Most of crude benzene refining devices in China adopt an acid washing process, and the amount of waste sulfuric acid generated every year is considerable, for example, about 1.6kt/a of waste sulfuric acid produced in Panzhi steel and about 3kt/a of the waste sulfuric acid produced in Jinpan steel are about 700t/a of a Jining coal chemical company. In the waste sulfuric acid, the sulfuric acid contains 40-60 wt% of sulfuric acid, benzene sulfonic acid, unsaturated resin, pyridine, quinoline, their homologues and other organic matters, and owing to the organic pigment and iron ion, the waste sulfuric acid is black and sticky. Therefore, if the crude benzene refining waste sulfuric acid can be well purified and utilized, not only resources are effectively utilized, but also considerable economic benefits, social benefits and environmental benefits are brought to enterprises.
The technical personnel begin to purify and recycle the crude benzene refining waste sulfuric acid, and the purification method of the crude benzene refining waste sulfuric acid in China mainly comprises a roasting method, an extraction-adsorption method, a thermal polymerization method and the like. Wherein, the roasting method has high energy consumption and large equipment investment; the extraction-adsorption method has difficulty in recovering the extractant; the thermal polymerization method has harsh reaction conditions, high equipment investment and high energy consumption, and the quality of the regenerated sulfuric acid is still poor; therefore, the technical problem to be solved in the current technical field is solved by designing a treatment process of the waste sulfuric acid, which has the advantages of simple process steps, environmental protection, low equipment investment, low energy consumption, high concentration of the treated sulfuric acid and low COD value.
The present invention focuses on this phenomenon and solves these problems by devising a process for treating spent sulfuric acid.
Disclosure of Invention
The invention aims to provide a treatment process of waste sulfuric acid, which aims to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
a treatment process of waste sulfuric acid comprises the following process steps: primary filtering, cooling and extracting, secondary filtering, tertiary filtering and high-temperature concentrating.
Further, the treatment process of the waste sulfuric acid comprises the following process steps:
(1) mixing waste sulfuric acid and deionized water according to a mass ratio of 1: 2-1: 4, uniformly mixing, pumping into a plate-and-frame filter press, and carrying out filter pressing to obtain primary filtered waste sulfuric acid;
(2) cooling and standing the waste sulfuric acid subjected to primary filtration for 2-3 h, and taking supernatant liquid as the cooled and extracted waste sulfuric acid;
(3) adding zinc hydroxide with the mass being 3-5 times that of the cooled and extracted waste sulfuric acid into the cooled and extracted waste sulfuric acid, uniformly mixing, heating to 65-75 ℃, stirring for 50-70 min at the speed of 400-600 r/min, naturally cooling to room temperature, pumping into a plate-and-frame filter press, and carrying out filter pressing to obtain secondarily filtered waste sulfuric acid;
(4) heating the waste sulfuric acid subjected to secondary filtration to 80-90 ℃ under the protection of argon, then introducing chlorine, adjusting the pH of the waste sulfuric acid subjected to secondary filtration to 5-9, stirring for 80-90 min at 400-600 r/min, naturally cooling to room temperature, continuously introducing chlorine for 0.5-0.7 h, stirring for 50-70 min at 400-600 r/min, pumping into a plate-and-frame filter press, and performing filter pressing to obtain waste sulfuric acid subjected to tertiary filtration of filtrate and filter residue zinc chloride pyridine complex salt;
(5) under the protection of argon, adding a sulfuric acid solution with the mass 0.6-0.8 times that of the waste sulfuric acid obtained by the third filtration, stirring for 2-4 hours at a speed of 400-600 r/min, and then heating and stirring for 3-4 hours to obtain treated sulfuric acid and tail gas.
Further, the waste sulfuric acid in the step (1) is waste sulfuric acid refined from crude benzene; the mass fraction of sulfuric acid in the waste sulfuric acid refined from crude benzene is 40-60%, and the COD value is 100000-300000 mg/L.
Further, the cooling temperature in the step (2) is 1-3 ℃.
Further, the flow rate of the chlorine gas in the step (4) is 800-15000L/h.
Further, the mass fraction of the sulfuric acid solution in the step (5) is 98%.
Further, the heating temperature in the step (5) is 130-140 ℃.
And (3) further, introducing the tail gas in the step (5) into a spray tower for spraying and removing.
Further, the temperature of the spray liquid in the spray tower is 60-80 ℃.
Further, the spraying liquid is a sodium hydroxide solution with the mass fraction of 20-30%.
Compared with the prior art, the invention has the following beneficial effects:
the treatment process of the waste sulfuric acid comprises the following process steps: primary filtering, cooling extraction, secondary filtering, tertiary filtering and high-temperature concentration; the primary filtration is to dilute the waste sulfuric acid and then filter to remove insoluble solid impurities to obtain the primary filtered waste sulfuric acid; cooling and extracting, namely cooling and extracting the waste sulfuric acid subjected to primary filtration to remove quinoline, and taking supernatant to obtain the cooled and extracted waste sulfuric acid; the secondary filtration is to add zinc hydroxide into the cooled and extracted waste sulfuric acid and then filter-press the mixture to obtain the secondarily filtered waste sulfuric acid and ferric hydroxide coarse material; the third filtration is to introduce chlorine into the waste sulfuric acid after the second filtration and then filter the waste sulfuric acid to obtain the waste sulfuric acid after the third filtration and zinc chloride pyridine complex salt; the high-temperature concentration is to add concentrated sulfuric acid into the waste sulfuric acid filtered for three times and then concentrate the mixture at high temperature to obtain treated sulfuric acid, and the tail gas is treated by spraying hot alkali liquor; the treatment process of the waste sulfuric acid has the advantages of simple process steps, environmental protection, low energy consumption, high concentration of the treated sulfuric acid and low COD value.
Firstly, zinc hydroxide reacts with iron ions in the cooled and extracted waste sulfuric acid to form iron hydroxide precipitate, so that residual iron ions can be effectively removed, and the concentration of sulfuric acid in the secondarily filtered waste sulfuric acid is increased; on the other hand, the alkaline zinc hydroxide can promote the hydrolysis of the high molecular unsaturated resin in the waste liquid after cooling extraction to form small molecular unsaturated alcohol and acid, which is favorable for the oxidative decomposition of organic matters in the waste sulfuric acid after secondary filtration in the third filtration.
Secondly, part of chlorine reacts with water in the waste liquid after secondary filtration to form hydrogen chloride and hypochlorous acid, and the hypochlorous acid oxidizes unsaturated alcohol and organic matters such as acid, aniline and phenol in the waste liquid after secondary filtration to form carbon dioxide, water, benzoquinone and hydrogen chloride, so that the COD value in the waste sulfuric acid after tertiary filtration is reduced; part of chlorine and hydrogen chloride react with zinc ions and pyridine in the waste liquid after secondary filtration to form zinc chloride pyridine complex salt which is insoluble in water, the zinc chloride pyridine complex salt can form zinc hydroxide by adding sodium hydroxide, and the zinc hydroxide can be recycled in secondary filtration for secondary utilization.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
To more clearly illustrate the process of the present invention, the following examples are provided to illustrate the process of the present invention, and the test methods for each index of the treated sulfuric acid prepared in the following examples are as follows:
COD value: the treated sulfuric acids obtained in the same mass of the examples and comparative examples were used to test the COD value according to HJ/T399.
Concentration of sulfuric acid: the same mass of treated sulfuric acid obtained in examples and comparative examples was taken, and the treated sulfuric acid was titrated with 1mol/L sodium hydroxide solution using phenolphthalein as an indicator, and the sulfuric acid concentration in the treated sulfuric acid was 1mol/L sodium hydroxide solution volume usage was 100% of the molar mass of sulfuric acid per mass of treated sulfuric acid.
And (3) zinc hydroxide content determination: taking the same mass of the zinc chloride pyridine complex salt obtained in the step (4) in the embodiments 1 to 3, adding a sodium hydroxide solution with a mass fraction of 40% and a mass of 0.3 times of that of the zinc chloride pyridine complex salt into the filter residue, stirring at 500r/min for 15min, standing for 1h, filtering, washing with deionized water for 3 times, filtering, drying at 40 ℃ for 2h to obtain a precipitate, and determining the content of zinc hydroxide according to Q/320681GSQ 11.
Example 1
(1) The mass fraction of sulfuric acid is 40%, COD value is 100000mg/L waste sulfuric acid refined from crude benzene and deionized water according to the mass ratio of 1: 2, uniformly mixing, pumping into a plate-and-frame filter press, and carrying out filter pressing to obtain primary filtered waste sulfuric acid;
(2) cooling the waste sulfuric acid subjected to primary filtration to 1 ℃, preserving heat and standing for 2 hours, and taking supernatant liquid as the cooled and extracted waste sulfuric acid;
(3) adding zinc hydroxide with the mass 3 times of that of the cooled and extracted waste sulfuric acid, uniformly mixing, heating to 65 ℃, stirring for 50min at the speed of 400r/min, naturally cooling to room temperature, pumping into a plate-and-frame filter press, and carrying out filter pressing to obtain secondarily filtered waste sulfuric acid;
(4) heating the waste sulfuric acid subjected to secondary filtration to 80 ℃ under the protection of argon, then introducing chlorine at 800L/h, adjusting the pH value of the waste sulfuric acid subjected to secondary filtration to 5, stirring for 80min at 400r/min, naturally cooling to room temperature, continuously introducing chlorine for 0.5h, stirring for 50min at 400r/min, pumping into a plate-and-frame filter press, and performing filter pressing to obtain waste sulfuric acid subjected to tertiary filtration of filtrate and filter residue zinc chloride pyridine complex salt;
(5) adding sulfuric acid solution with mass fraction of 98% and mass of 0.6 times of that of the waste sulfuric acid filtered for three times under the protection of argon, stirring for 2 hours at 400r/min, then heating to 130 ℃, continuously stirring for 3 hours to obtain treated sulfuric acid and tail gas, and introducing the tail gas into a spray tower which takes 20% sodium hydroxide solution at 60 ℃ as spray liquid to spray and remove the tail gas.
Example 2
(1) The mass fraction of sulfuric acid is 50%, the COD value is 200000mg/L, the waste sulfuric acid refined from crude benzene and deionized water are mixed according to the mass ratio of 1: 3, uniformly mixing, pumping into a plate-and-frame filter press, and carrying out filter pressing to obtain primary filtered waste sulfuric acid;
(2) cooling the once filtered waste sulfuric acid to 2 ℃, preserving heat and standing for 2.5 hours, and taking supernatant as the cooled and extracted waste sulfuric acid;
(3) adding zinc hydroxide with the mass being 4 times that of the cooled and extracted waste sulfuric acid into the cooled and extracted waste sulfuric acid, uniformly mixing, heating to 70 ℃, stirring at 500r/min for 60min, naturally cooling to room temperature, pumping into a plate-and-frame filter press, and carrying out filter pressing to obtain secondarily filtered waste sulfuric acid;
(4) heating the waste sulfuric acid subjected to secondary filtration to 85 ℃ under the protection of argon, then introducing chlorine at 7900L/h, adjusting the pH value of the waste sulfuric acid subjected to secondary filtration to 7, stirring for 85min at 500r/min, naturally cooling to room temperature, continuously introducing chlorine for 0.6h, stirring for 60min at 500r/min, pumping into a plate-and-frame filter press, and performing filter pressing to obtain waste sulfuric acid subjected to tertiary filtration of filtrate and filter residue zinc chloride pyridine complex salt;
(5) adding sulfuric acid solution with mass fraction of 98% which is 0.7 times of the mass of the waste sulfuric acid filtered for three times under the protection of argon gas, stirring for 3 hours at 500r/min, then heating to 135 ℃, continuously stirring for 3.5 hours to obtain treated sulfuric acid and tail gas, and introducing the tail gas into a spray tower which takes 25% of sodium hydroxide solution at 70 ℃ as spray liquid to spray and remove the tail gas.
Example 3
(1) 60 percent of sulfuric acid by mass and 300000mg/L of COD value of crude benzene refined waste sulfuric acid and deionized water are mixed according to the mass ratio of 1: 4, uniformly mixing, pumping into a plate-and-frame filter press, and carrying out filter pressing to obtain primary filtered waste sulfuric acid;
(2) cooling the primarily filtered waste sulfuric acid to 3 ℃, preserving heat and standing for 3 hours, and taking supernatant as the cooled and extracted waste sulfuric acid;
(3) adding zinc hydroxide with the mass 5 times of that of the cooled and extracted waste sulfuric acid into the cooled and extracted waste sulfuric acid, uniformly mixing, heating to 75 ℃, stirring at 600r/min for 70min, naturally cooling to room temperature, pumping into a plate-and-frame filter press, and carrying out filter pressing to obtain secondarily filtered waste sulfuric acid;
(4) heating the waste sulfuric acid subjected to secondary filtration to 90 ℃ under the protection of argon, introducing chlorine at 15000L/h, adjusting the pH value of the waste sulfuric acid subjected to secondary filtration to 9, stirring for 90min at 600r/min, naturally cooling to room temperature, continuously introducing chlorine for 0.7h, stirring for 70min at 600r/min, pumping into a plate-and-frame filter press, and performing filter pressing to obtain waste sulfuric acid subjected to tertiary filtration of filtrate and filter residue zinc chloride pyridine complex salt;
(5) adding sulfuric acid solution with mass fraction of 98% and mass of 0.8 times of that of the waste sulfuric acid filtered for three times under the protection of argon, stirring for 4 hours at 600r/min, then heating to 140 ℃, continuing stirring for 4 hours to obtain treated sulfuric acid and tail gas, and introducing the tail gas into a spray tower which takes 30% sodium hydroxide solution at 80 ℃ as spray liquid to spray and remove the tail gas.
Examples of effects
Table 1 below gives the results of the analysis of the COD value and the sulfuric acid concentration of the treated sulfuric acid prepared in examples 1 to 3 of the present invention.
TABLE 1
| Example 1 | Example 2 | Example 3 | |
| COD value (mg/L) | 25 | 20 | 32 |
| Sulfuric acid concentration (%) | 95.46 | 96.53 | 96.25 |
| Zinc hydroxide content (%) | 98.12 | 98.86 | 98.35 |
From table 1, it can be seen that the treated sulfuric acids prepared in examples 1, 2 and 3 have a low COD value and a high sulfuric acid concentration, and the zinc chloride pyridine complex salt obtained in step (4) is subjected to alkaline decomposition to obtain zinc hydroxide, which is then fed to step (3) for reuse.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (10)
1. The treatment process of the waste sulfuric acid is characterized by comprising the following process steps of: primary filtering, cooling and extracting, secondary filtering, tertiary filtering and high-temperature concentrating.
2. The process for treating waste sulfuric acid as claimed in claim 1, wherein the process for treating waste sulfuric acid comprises the following process steps:
(1) mixing waste sulfuric acid and deionized water according to a mass ratio of 1: 2-1: 4, uniformly mixing, pumping into a plate-and-frame filter press, and carrying out filter pressing to obtain primary filtered waste sulfuric acid;
(2) cooling and standing the waste sulfuric acid subjected to primary filtration for 2-3 h, and taking supernatant liquid as the cooled and extracted waste sulfuric acid;
(3) adding zinc hydroxide with the mass being 3-5 times that of the cooled and extracted waste sulfuric acid into the cooled and extracted waste sulfuric acid, uniformly mixing, heating to 65-75 ℃, stirring for 50-70 min at the speed of 400-600 r/min, naturally cooling to room temperature, pumping into a plate-and-frame filter press, and carrying out filter pressing to obtain secondarily filtered waste sulfuric acid;
(4) heating the waste sulfuric acid subjected to secondary filtration to 80-90 ℃ under the protection of argon, then introducing chlorine, adjusting the pH value of the waste sulfuric acid subjected to secondary filtration to 5-9, stirring for 80-90 min at 400-600 r/min, naturally cooling to room temperature, continuously introducing chlorine for 0.5-0.7 h, stirring for 50-70 min at 400-600 r/min, pumping into a plate-and-frame filter press, and carrying out filter pressing to obtain waste sulfuric acid subjected to tertiary filtration of filtrate and filter residue zinc chloride pyridine complex salt;
(5) under the protection of argon, adding a sulfuric acid solution with the mass 0.6-0.8 times that of the waste sulfuric acid obtained by the third filtration, stirring for 2-4 hours at a speed of 400-600 r/min, and then heating and stirring for 3-4 hours to obtain treated sulfuric acid and tail gas.
3. The process according to claim 2, wherein the waste sulfuric acid obtained in step (1) is a waste sulfuric acid obtained by refining crude benzene; the mass fraction of sulfuric acid in the waste sulfuric acid refined from crude benzene is 40-60%, and the COD value is 100000-300000 mg/L.
4. The process according to claim 2, wherein the cooling temperature in the step (2) is 1-3 ℃.
5. The process according to claim 2, wherein the flow rate of the chlorine gas in the step (4) is 800-15000L/h.
6. The process of claim 2, wherein the mass fraction of the sulfuric acid solution in the step (5) is 98%.
7. The process according to claim 2, wherein the heating temperature in the step (5) is 130-140 ℃.
8. The process of claim 2, wherein the tail gas in the step (5) is removed by spraying in a spray tower.
9. The process according to claim 8, wherein the temperature of the spray liquid in the spray tower is 60-80 ℃.
10. The process for treating waste sulfuric acid as claimed in claim 9, wherein the spraying liquid is a sodium hydroxide solution with a mass fraction of 20-30%.
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| EP1112997A2 (en) * | 1999-12-28 | 2001-07-04 | Mitsubishi Chemical Corporation | Process for producing diaryl carbonate |
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| CN103205271A (en) * | 2012-01-12 | 2013-07-17 | 易高环保能源研究院有限公司 | Method for hydrogenation of high temperature coal tar to produce mesophase pitch |
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| CN109368668A (en) * | 2018-11-26 | 2019-02-22 | 四川大学 | A kind of Waste Sulfuric Acid processing method |
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2022
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| EP1112997A2 (en) * | 1999-12-28 | 2001-07-04 | Mitsubishi Chemical Corporation | Process for producing diaryl carbonate |
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