CN115124179B - Treatment process of waste sulfuric acid - Google Patents
Treatment process of waste sulfuric acid Download PDFInfo
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- CN115124179B CN115124179B CN202210906174.9A CN202210906174A CN115124179B CN 115124179 B CN115124179 B CN 115124179B CN 202210906174 A CN202210906174 A CN 202210906174A CN 115124179 B CN115124179 B CN 115124179B
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- 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
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; filtering and pressing the waste sulfuric acid to remove solid impurities to obtain waste sulfuric acid which is filtered once; then the filtered waste sulfuric acid is cooled and extracted to remove quinoline, so as to obtain cooled and extracted waste sulfuric acid; then zinc hydroxide is added into the cooled and extracted waste sulfuric acid for filter pressing, so as to obtain secondary filtered waste sulfuric acid; then introducing chlorine into the secondarily filtered waste sulfuric acid for filtering to obtain tertiary filtered waste sulfuric acid and filter residue zinc chloride pyridine complex salt, decomposing the zinc chloride pyridine complex salt and alkali to obtain zinc hydroxide, and putting the zinc hydroxide into secondary filtering again for use; 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 waste liquid produced in the course of pickling benzene processing in coking plant. Most crude benzene refining devices in China adopt an acid washing process, and the amount of waste sulfuric acid generated each year is considerable, for example, about 1.6kt/a of waste sulfuric acid produced by Pan steel and about 3kt/a of Jining coal chemical company are about 700t/a. The waste sulfuric acid contains 40-60% sulfuric acid, benzenesulfonic acid, unsaturated resin, pyridine, quinoline and its homologs, and other organic matters, and its appearance is black and viscous due to the existence of organic pigment and iron ions. Therefore, if the waste sulfuric acid from crude benzene refining can be well purified and utilized, not only the resources are effectively utilized, but also considerable economic, social and environmental benefits are brought to enterprises.
Therefore, technicians begin to purify and recycle the crude benzene refined waste sulfuric acid, and the purification methods of the crude benzene refined waste sulfuric acid in China mainly comprise 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 difficult recovery of the extractant; the thermal polymerization method has the advantages of harsh reaction conditions, high equipment investment, high energy consumption and poor quality of regenerated sulfuric acid; therefore, the design of the treatment process of the waste sulfuric acid with simple process steps, environmental protection, low equipment investment, low energy consumption, high concentration of the treated sulfuric acid and low COD value becomes a technical problem to be solved urgently in the current technical field.
The present invention focuses on this phenomenon and solves these problems by designing 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 process for treating waste sulfuric acid, comprising the following process steps: primary filtering, cooling extraction, secondary filtering, tertiary filtering and high-temperature concentration.
Further, the treatment process of the waste sulfuric acid comprises the following process steps:
(1) Waste sulfuric acid and deionized water are mixed according to the mass ratio of 1: 2-1: 4, uniformly mixing, pumping into a plate-and-frame filter press for filter pressing to obtain waste sulfuric acid which is filtered once;
(2) Cooling and standing the waste sulfuric acid subjected to primary filtration for 2-3 hours, and taking the supernatant as the waste sulfuric acid subjected to cooling and extraction;
(3) Adding zinc hydroxide 3-5 times of the mass 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 400-600 r/min, naturally cooling to room temperature, pumping into a plate-and-frame filter press for filter pressing, and obtaining secondary filtered waste sulfuric acid;
(4) Under the protection of argon, heating the secondarily filtered waste sulfuric acid to 80-90 ℃, then introducing chlorine gas, adjusting the pH of the secondarily filtered waste sulfuric acid to 5-9, stirring for 80-90 min at 400-600 r/min, naturally cooling to room temperature, continuously introducing chlorine gas for 0.5-0.7 h, stirring for 50-70 min at 400-600 r/min, pumping into a plate-and-frame filter press for filter pressing, and obtaining the waste sulfuric acid and filter residue zinc chloride pyridine complex salt of the tertiary filtration of the filtrate;
(5) Under the protection of argon, adding sulfuric acid solution with the mass of 0.6-0.8 times of that of the waste sulfuric acid filtered for three times into the waste sulfuric acid filtered for three times, stirring for 2-4 hours at the speed of 400-600 r/min, and then heating and stirring for 3-4 hours to obtain the treated sulfuric acid and tail gas.
Further, the waste sulfuric acid in the step (1) is waste sulfuric acid refined by crude benzene; the mass fraction of sulfuric acid in the waste sulfuric acid refined by the crude benzene is 40% -60%, and the COD value is 100000 ～ 300000mg/L.
Further, the cooling temperature in the step (2) is 1-3 ℃.
Further, the flow rate of the chlorine 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 ℃.
Further, the tail gas in the step (5) is introduced into a spray tower for spray removal.
Further, the temperature of the spray liquid in the spray tower is 60-80 ℃.
Further, the spray liquid is 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 and extracting, secondary filtering, tertiary filtering and high-temperature concentrating; the primary filtration is to dilute the waste sulfuric acid and then filter the diluted waste sulfuric acid to remove indissolvable solid impurities, so as to obtain the primary filtered waste sulfuric acid; the cooling extraction is to cool and extract the waste sulfuric acid filtered at one time to remove quinoline, and take the supernatant to obtain the waste sulfuric acid of cooling extraction; the secondary filtration is to add zinc hydroxide into the cooled and extracted waste sulfuric acid and then filter-press the mixture to obtain secondary filtered waste sulfuric acid and coarse ferric hydroxide; the third filtering is to introduce chlorine into the waste sulfuric acid after the second filtering, and then filter the waste sulfuric acid to obtain the waste sulfuric acid and zinc chloride pyridine complex salt after the third filtering; the high-temperature concentration is to add concentrated sulfuric acid into the waste sulfuric acid filtered for three times, then concentrate the waste sulfuric acid at high temperature to obtain treated sulfuric acid, and treat tail gas 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 ferric ions in the cooled and extracted waste sulfuric acid to form ferric hydroxide precipitate, so that residual ferric ions can be effectively removed, and the concentration of sulfuric acid in the secondarily filtered waste sulfuric acid is improved; on the other hand, the alkaline zinc hydroxide can promote the hydrolysis of high molecular unsaturated resin in the cooled extracted waste liquid to form small molecular unsaturated alcohol and acid, which is favorable for the oxidative decomposition of organic matters in the waste sulfuric acid filtered for the second time in the third filtering.
Secondly, partial chlorine reacts with water in the secondary filtered waste liquid to form hydrogen chloride and hypochlorous acid, and the hypochlorous acid oxidizes unsaturated alcohols, acids, aniline, phenol and other organic matters in the secondary filtered waste liquid to form carbon dioxide, water, benzoquinone and hydrogen chloride, so that the COD value in the waste sulfuric acid of the tertiary filtration is reduced; part of chlorine and hydrogen chloride react with zinc ions and pyridine in the secondary filtered waste liquid to form water-insoluble zinc chloride pyridine complex salt, and the zinc chloride pyridine complex salt can be added with sodium hydroxide to form zinc hydroxide, and the zinc hydroxide can be recycled to secondary filtration for secondary utilization.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In order to more clearly illustrate the method provided by the invention, the following examples are used to describe the method for testing each index of the treated sulfuric acid prepared in the following examples as follows:
COD value: the treated sulfuric acid prepared in examples and comparative examples of the same quality was taken and tested for COD value according to HJ/T399.
Sulfuric acid concentration: the treated sulfuric acid obtained in the examples and comparative examples of the same mass was titrated with 1mol/L sodium hydroxide solution using phenolphthalein as an indicator, and the sulfuric acid concentration=1 mol/L sodium hydroxide solution volume amount in the treated sulfuric acid was 100% of the molar mass of the sulfuric acid per the mass of the treated sulfuric acid.
And (3) measuring the content of zinc hydroxide: taking the zinc pyridine complex salt of the filter residue obtained in the step (4) in the examples 1 to 3 with the same mass, adding a sodium hydroxide solution with the mass fraction of 40% which is 0.3 times that of the zinc pyridine complex salt of the filter residue, stirring for 15min at 500r/min, standing for 1h for filtering, washing 3 times with deionized water, filtering, and baking at 40 ℃ for 2h to obtain a precipitate, and determining the zinc hydroxide content according to Q/320681GSQ 11.
Example 1
(1) The method comprises the steps of (1) mixing waste sulfuric acid purified by crude benzene with sulfuric acid mass fraction of 40% and COD value of 100000mg/L with deionized water: 2, uniformly mixing, pumping into a plate-and-frame filter press for filter pressing to obtain waste sulfuric acid which is filtered once;
(2) Cooling the waste sulfuric acid subjected to primary filtration to 1 ℃, preserving heat and standing for 2 hours, and taking the supernatant as the waste sulfuric acid subjected to cooling extraction;
(3) Adding zinc hydroxide 3 times of the cooled and extracted waste sulfuric acid, uniformly mixing, heating to 65 ℃, stirring for 50min at 400r/min, naturally cooling to room temperature, pumping into a plate-and-frame filter press for filter pressing to obtain secondary filtered waste sulfuric acid;
(4) Under the protection of argon, heating the secondarily filtered waste sulfuric acid to 80 ℃, then introducing chlorine gas at 800L/h, adjusting the pH of the secondarily filtered waste sulfuric acid to 5, stirring for 80min at 400r/min, naturally cooling to room temperature, continuously introducing chlorine gas for 0.5h, stirring for 50min at 400r/min, pumping into a plate-and-frame filter press, and performing filter pressing to obtain the waste sulfuric acid and filter residue zinc chloride pyridine complex salt of the tertiary filtration of the filtrate;
(5) Under the protection of argon, adding a sulfuric acid solution with the mass fraction of 98% which is 0.6 times of that of the waste sulfuric acid filtered for three times into the waste sulfuric acid filtered for three times, stirring for 2 hours at 400r/min, then heating to 130 ℃, continuing stirring for 3 hours to obtain treated sulfuric acid and tail gas, and introducing the tail gas into a spray tower with a 20% sodium hydroxide solution at 60 ℃ as a spray liquid for spray removal.
Example 2
(1) The method comprises the steps of (1) mixing waste sulfuric acid purified by crude benzene with sulfuric acid of which the mass fraction is 50% and the COD value is 200000mg/L with deionized water according to the mass ratio of 1:3, uniformly mixing, pumping into a plate-and-frame filter press for filter pressing to obtain waste sulfuric acid subjected to primary filtration;
(2) Cooling the waste sulfuric acid subjected to primary filtration to 2 ℃, keeping the temperature and standing for 2.5 hours, and taking the supernatant as the waste sulfuric acid subjected to cooling extraction;
(3) Adding zinc hydroxide with the mass 4 times of that of the cooled and extracted waste sulfuric acid, uniformly mixing, heating to 70 ℃, stirring for 60min at 500r/min, naturally cooling to room temperature, pumping into a plate-and-frame filter press for filter pressing to obtain secondary filtered waste sulfuric acid;
(4) Under the protection of argon, heating the secondarily filtered waste sulfuric acid to 85 ℃, then introducing chlorine gas at 7900L/h, adjusting the pH of the secondarily filtered waste sulfuric acid to 7, stirring for 85min at 500r/min, naturally cooling to room temperature, continuously introducing chlorine gas for 0.6h, stirring for 60min at 500r/min, pumping into a plate-and-frame filter press, and performing filter pressing to obtain the waste sulfuric acid and filter residue zinc chloride pyridine complex salt of the tertiary filtration of the filtrate;
(5) Under the protection of argon, adding a sulfuric acid solution with the mass fraction of 98% which is 0.7 times of that of the waste sulfuric acid filtered for three times into the waste sulfuric acid filtered for three times, stirring for 3 hours at 500r/min, then heating to 135 ℃, continuing stirring for 3.5 hours to obtain treated sulfuric acid and tail gas, and introducing the tail gas into a spray tower with a 25% sodium hydroxide solution at 70 ℃ as a spray liquid for spray removal.
Example 3
(1) The method comprises the steps of (1) mixing waste sulfuric acid purified by crude benzene with sulfuric acid mass fraction of 60% and COD value of 300000mg/L with deionized water: 4, uniformly mixing, pumping into a plate-and-frame filter press for filter pressing to obtain waste sulfuric acid which is filtered once;
(2) Cooling the waste sulfuric acid subjected to primary filtration to 3 ℃, preserving heat and standing for 3 hours, and taking the supernatant as the waste sulfuric acid subjected to cooling extraction;
(3) Adding zinc hydroxide with the mass 5 times of that of the cooled and extracted waste sulfuric acid, uniformly mixing, heating to 75 ℃, stirring for 70min at 600r/min, naturally cooling to room temperature, pumping into a plate-and-frame filter press for filter pressing to obtain secondary filtered waste sulfuric acid;
(4) Under the protection of argon, heating the secondarily filtered waste sulfuric acid to 90 ℃, then introducing chlorine gas at 15000L/h, adjusting the pH of the secondarily filtered waste sulfuric acid to 9, stirring for 90min at 600r/min, naturally cooling to room temperature, continuously introducing chlorine gas for 0.7h, stirring for 70min at 600r/min, pumping into a plate-and-frame filter press, and performing filter pressing to obtain the waste sulfuric acid and filter residue zinc chloride pyridine complex salt of the filtrate which are filtered for three times;
(5) Under the protection of argon, adding a sulfuric acid solution with the mass fraction of 98% which is 0.8 times of that of the waste sulfuric acid filtered for three times into the waste sulfuric acid filtered for three times, 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 taking a 30% sodium hydroxide solution at 80 ℃ as a spray liquid for spray removal.
Effect example
The following table 1 shows the analysis results of the COD value and sulfuric acid concentration of the treated sulfuric acid prepared by using 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 was found that the treated sulfuric acid obtained in examples 1, 2 and 3 had a low COD value and a high sulfuric acid concentration, and that the zinc chloride pyridine complex salt of the residue obtained in step (4) could be subjected to alkali decomposition to obtain zinc hydroxide and recycled in step (3).
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 characteristics 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 (9)
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;
the primary filtration is to dilute the waste sulfuric acid and then filter the diluted waste sulfuric acid to remove indissolvable solid impurities, so as to obtain the primary filtered waste sulfuric acid;
the treatment process of the waste sulfuric acid comprises the following process steps:
(1) Waste sulfuric acid and deionized water are mixed according to the mass ratio of 1: 2-1: 4, uniformly mixing, pumping into a plate-and-frame filter press for filter pressing to obtain waste sulfuric acid which is filtered once;
the waste sulfuric acid is waste sulfuric acid refined by crude benzene;
(2) Cooling and standing the waste sulfuric acid subjected to primary filtration for 2-3 hours, cooling and extracting to remove quinoline, and taking the supernatant as the waste sulfuric acid subjected to cooling and extracting;
(3) Adding zinc hydroxide 3-5 times of the mass 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 400-600 r/min, naturally cooling to room temperature, pumping into a plate-and-frame filter press for filter pressing, and obtaining secondary filtered waste sulfuric acid and coarse ferric hydroxide;
(4) Under the protection of argon, heating the secondarily filtered waste sulfuric acid to 80-90 ℃, then introducing chlorine gas, adjusting the pH of the secondarily filtered waste sulfuric acid to 5-9, stirring for 80-90 min at 400-600 r/min, naturally cooling to room temperature, continuously introducing chlorine gas for 0.5-0.7 h, stirring for 50-70 min at 400-600 r/min, pumping into a plate-and-frame filter press for filter pressing, and obtaining the waste sulfuric acid and filter residue zinc chloride pyridine complex salt of the tertiary filtration of the filtrate;
(5) Under the protection of argon, adding sulfuric acid solution with the mass of 0.6-0.8 times of that of the waste sulfuric acid filtered for three times into the waste sulfuric acid filtered for three times, stirring for 2-4 hours at the speed of 400-600 r/min, and then heating and stirring for 3-4 hours to obtain the treated sulfuric acid and tail gas.
2. The process for treating waste sulfuric acid according to claim 1, wherein the mass fraction of sulfuric acid in the waste sulfuric acid purified from crude benzene in the step (1) is 40% -60%, and the COD value is 100000 ～ 300000mg/L.
3. The process according to claim 1, wherein the cooling temperature in the step (2) is 1 to 3 ℃.
4. The process according to claim 1, wherein the flow rate of the chlorine gas in the step (4) is 800 to 15000L/h.
5. The process for treating waste sulfuric acid according to claim 1, wherein the mass fraction of the sulfuric acid solution in the step (5) is 98%.
6. The process according to claim 1, wherein the heating temperature in the step (5) is 130 to 140 ℃.
7. The process for treating waste sulfuric acid according to claim 1, wherein the tail gas in the step (5) is introduced into a spray tower for spray removal.
8. The process for treating waste sulfuric acid as claimed in claim 7, wherein the temperature of the spray liquid in the spray tower is 60-80 ℃.
9. The process for treating waste sulfuric acid according to claim 8, wherein the spray liquid is a sodium hydroxide solution with a mass fraction of 20-30%.
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| DE606235C (en) * | 1931-12-19 | 1934-11-28 | Metallgesellschaft Ag | Process for the production of sulfuric acid by the contact process |
| EP1112997B1 (en) * | 1999-12-28 | 2009-05-13 | Mitsubishi Chemical Corporation | Process for producing diaryl carbonate |
| CN1149174C (en) * | 2000-07-18 | 2004-05-12 | 本溪钢铁(集团)有限责任公司 | Method for preparing sulfuric acid by incineration of refined benzene regeneration acid |
| CN101824530A (en) * | 2010-04-08 | 2010-09-08 | 白向南 | Process for roasting chromite resources in ring kiln through pure oxygen by using low-temperature method and harmlessly and deeply utilizing chromium residue |
| CN103205271B (en) * | 2012-01-12 | 2016-03-09 | 易高环保能源研究院有限公司 | Hydrogenation of high temperature coal tar produces the method for mesophase pitch |
| CN105084607B (en) * | 2015-09-17 | 2017-05-31 | 博天环境集团股份有限公司 | A kind of biochemical pre-treating method of acrylic ester wastewater |
| CN109368668B (en) * | 2018-11-26 | 2021-01-15 | 四川大学 | Waste sulfuric acid treatment method |
| CN111874874A (en) * | 2020-07-28 | 2020-11-03 | 安徽东至广信农化有限公司 | Waste sulfuric acid recovery and concentration process |
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