CN115504499A - Method for refining gypsum from chemical wastewater containing sulfuric acid and sulfate - Google Patents
Method for refining gypsum from chemical wastewater containing sulfuric acid and sulfate Download PDFInfo
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- CN115504499A CN115504499A CN202211297380.0A CN202211297380A CN115504499A CN 115504499 A CN115504499 A CN 115504499A CN 202211297380 A CN202211297380 A CN 202211297380A CN 115504499 A CN115504499 A CN 115504499A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
- C04B22/08—Acids or salts thereof
- C04B22/14—Acids or salts thereof containing sulfur in the anion, e.g. sulfides
- C04B22/142—Sulfates
- C04B22/143—Calcium-sulfate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
Abstract
The invention belongs to the field of chemical wastewater treatment, relates to treatment of chemical wastewater containing sulfuric acid and sulfate, and particularly relates to a method for refining gypsum from the chemical wastewater containing the sulfuric acid and the sulfate. The invention applies the ozone advanced oxidation method to remove the pollutants in the wastewater, can ensure that the effluent of the chemical wastewater containing sulfuric acid and sulfate reaches the standard after the subsequent process, realizes the refining and purification to obtain the gypsum, and conforms to the standard of GB/T21371-2008 (the industrial by-product gypsum used in cement) as a cement speed regulator. The process method is efficient and stable, is simple and convenient to operate, treats pollution, simultaneously obtains comprehensive utilization, and has good environmental protection effect and economic benefit.
Description
Technical Field
The invention belongs to the field of chemical wastewater treatment, relates to treatment of chemical wastewater containing sulfuric acid and sulfate, and particularly relates to a method for refining gypsum from the chemical wastewater containing sulfuric acid and sulfate.
Background
The existing methods for treating wastewater containing sulfuric acid and sulfate mainly comprise a chemical precipitation method, an ion exchange method and an anaerobic decomposition method. Among them, the chemical precipitation method has the advantages of simple process flow, convenient operation and mature technology, and is one of the most common methods.
The chemical precipitation method mainly utilizes calcium oxide, calcium chloride, calcium hydroxide, barium chloride and the like to react with sulfate radicals to generate precipitates;
the ion exchange method mainly utilizes adsorption and exchange of sulfate radicals by anion resin. The disadvantages are that the investment cost of the ion exchange reactor is high and the requirement on resin is high;
the anaerobic decomposition method utilizes the sulfuric acid wastewater to flow back to the anoxic zone through the anaerobic reaction, the anoxic reaction and the aerobic reaction to generate methane and H 2 S, CN110316825A mentioned in patent publication mentions that after pH and water temperature of wastewater containing sulfate radicals are adjusted, methane gas is generated through anaerobic reaction, and then H is generated through anoxic and aerobic reaction 2 S is collected with NaOH solution for industrial use. The disadvantages are that the sulfate reducing bacteria consume a long time for culturing the desulfurization microorganisms, and the retention time of the wastewater in the anaerobic tank is 3-10 days, so that the retention time is long.
Some companies propose direct electrolysis, and patent CN106966469A mentions that a lead sheet is used as an anode, and an inert electrode is used as a cathode to perform an electrolysis reaction to generate PbSO 4 And (4) filtering the precipitate.
Therefore, there is a need to develop a method for efficiently and stably treating sulfuric acid-containing chemical wastewater and refining gypsum.
Disclosure of Invention
The invention aims to provide a method for refining gypsum from chemical wastewater containing sulfuric acid and sulfate, which not only removes pollutants in the wastewater, but also ensures that the effluent of the chemical wastewater containing sulfuric acid and sulfate reaches the standard through subsequent processes, and realizes refining and purification to obtain gypsum. The process method is efficient and stable, is simple and convenient to operate, has excellent product quality, and has good environmental protection effect and economic benefit.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for refining gypsum from chemical wastewater containing sulfuric acid and sulfate comprises the following steps:
(1) Adding hydrogen peroxide into chemical wastewater containing sulfuric acid and sulfate, and stirring for reaction;
(2) Adjusting the pH of the water treated in the step (1) to 4-5 by using calcium hydroxide;
(3) the water treated in the step (2) enters an ozone reactor to carry out ozone oxidation reaction;
(4) Adding alkali into the water treated in the step (3) to adjust the pH value to 8-9;
(5) The water treated in the step (4) enters an ozone reactor, and the ozone oxidation reaction is continuously carried out;
(6) And (4) respectively carrying out filter pressing, washing and drying on the water treated in the step (5) to obtain white crystals, namely the refined gypsum.
Preferably, the concentration of the sulfuric acid in the chemical wastewater containing sulfuric acid and sulfate in the step (1) is 2-10%.
Preferably, the concentration of the hydrogen peroxide in the step (1) is 27.5%;
the adding amount of the hydrogen peroxide in the step (1) is 10-50% of the weight of COD in the chemical wastewater containing sulfuric acid and sulfate.
Preferably, the stirring reaction time of the step (1) is 1h-2h.
Preferably, the calcium hydroxide in the step (2) is in a 30% suspension.
Preferably, the catalyst for the ozone oxidation reaction in the step (3) is a SAO 3-II series high-efficiency ozone catalyst.
Preferably, the ozone oxidation reaction time in the step (3) is 1-2h.
Preferably, the alkali in the step (4) is a 30% calcium hydroxide suspension.
Preferably, the catalyst for the ozone oxidation reaction in the step (5) is a SAO 3-II series high-efficiency ozone catalyst.
Preferably, the ozone oxidation reaction time in the step (5) is 0.5-1h.
And (6) allowing the pressure filtration filtrate to enter a normal sewage treatment system.
The invention has the following beneficial effects:
(1) The process method is simple and convenient to operate, stable in effect, environment-friendly and efficient.
(2) The invention can obtain refined gypsum, has higher recovery value, realizes resource recycling, can be used as a cement speed regulator, and meets the standard of GB/T21371-2008 (industrial by-product gypsum used in cement) as the cement speed regulator.
(3) The treatment method has good comprehensive treatment effect, and the application of the ozone advanced oxidation method not only can remove pollutants in the wastewater, but also can ensure that the effluent of the chemical wastewater containing sulfuric acid and sulfate reaches the standard through the subsequent process, so that the refining and purification of the gypsum are prepared, the pollution is treated, and the comprehensive utilization is realized, and the treatment method has good environmental protection effect and economic benefit.
Drawings
FIG. 1 is a picture of white crystals before drying;
fig. 2 is a picture of white crystals after drying.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in 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.
A method for refining gypsum from chemical wastewater containing sulfuric acid and sulfate comprises the following steps:
(1) Taking chemical wastewater containing sulfuric acid and sulfate, adding hydrogen peroxide with the weight of 10-50% of COD, and stirring for reaction for 1-2 hours;
(2) Adjusting the pH of the water treated in the step (1) to 4-5 by using calcium hydroxide;
(3) The water treated in the step (2) enters an ozone reactor to carry out direct ozone oxidation reaction for 1-2 hours, wherein the catalyst of the ozone oxidation reaction is SAO 3-II series high-efficiency ozone catalyst which is a commercial product;
(4) Adding alkali into the water treated in the step (3) to adjust the PH value to 8-9;
(5) The water treated in the step (4) enters an ozone reactor to carry out advanced ozone oxidation reaction for 0.5 to 1 hour, and the catalyst of the ozone oxidation reaction is SAO 3-II series high-efficiency ozone catalyst which is a commercial product;
(6) And (4) respectively carrying out filter pressing, washing and drying on the water treated in the step (5) to obtain white crystals. Namely the refined gypsum. Meanwhile, filter-pressing filtrate enters a normal sewage treatment system.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Example 1
Sulfuric acid mother liquor wastewater of a certain Shandong factory, and raw water quality: COD was 3425mg/L, sulfuric acid content was 9.5%, TDS (total dissolved solids) was 143350mg/L.
The method for treating the wastewater containing sulfuric acid and sulfate comprises the following steps:
(1) Adding 27.5% (mass fraction) 1050mg/L hydrogen peroxide into chemical wastewater containing sulfuric acid and sulfate, and stirring for reacting for 2 hours;
(2) Adjusting the pH of the water treated in the step (1) to 4 by using calcium hydroxide;
(3) The water treated in the step (2) enters an ozone reactor to carry out direct ozone oxidation reaction for 1.5 hours, and the catalyst of the ozone oxidation reaction is SAO 3-II series high-efficiency ozone catalyst which is a commercial product;
(4) Adding alkali into the water treated in the step (3) to adjust the pH value to 8.5;
(5) The water treated in the step (4) enters an ozone reactor, and continues to carry out advanced ozone oxidation reaction for 0.5 hour, wherein the catalyst of the ozone oxidation reaction is SAO 3-II series high-efficiency ozone catalyst which is a commercial product;
(6) And (3) respectively carrying out filter pressing, washing and drying on the water treated in the step (5) to obtain white crystals, namely refined gypsum, wherein the picture distribution of the white crystals before and after drying is shown in figures 1 and 2. Meanwhile, filter-pressing filtrate enters a normal sewage treatment system.
The white crystals finally obtained were taken for purity determination. The test was repeated three times, and the final white crystal was calcium sulfate crystal having an average purity of 78% or more. Through cement tests, the type I portland cement prepared by replacing dihydrate gypsum meets the standard of GB/T21371-2008 (industrial by-product gypsum used in cement) as a cement speed regulator.
Example 2
Sulfuric acid mother liquor wastewater of a certain Shandong factory, and the quality of raw water: COD was 3425mg/L, sulfuric acid content was 9.5%, TDS (total dissolved solids) was 143350mg/L.
The method for treating the wastewater containing sulfuric acid and sulfate comprises the following steps:
(1) Adding 27.5% (mass fraction) 1050mg/L hydrogen peroxide into chemical wastewater containing sulfuric acid and sulfate, and stirring for reacting for 2 hours;
(2) Adjusting the pH of the water treated in the step (1) to 4.5 by using calcium hydroxide;
(3) The water treated in the step (2) enters an ozone reactor for direct oxidation reaction for 1 hour, and the catalyst of the ozone oxidation reaction is SAO 3-II series high-efficiency ozone catalyst which is a commercial product;
(4) Adding alkali into the water treated in the step (3) to adjust the pH value to 9;
(5) The water treated in the step (4) enters an ozone reactor, and continues to carry out advanced ozone oxidation reaction for 0.5 hour, wherein the catalyst of the ozone oxidation reaction is SAO 3-II series high-efficiency ozone catalyst which is a commercial product;
(6) And (4) respectively carrying out filter pressing, washing and drying on the water treated in the step (5) to obtain white crystals, namely the refined gypsum. Meanwhile, filter-pressing filtrate enters a normal sewage treatment system.
The final white crystals were taken for purity. The test is repeated three times, and the final white crystal is calcium sulfate crystal with average purity of more than 76%. Through cement tests, the type I portland cement prepared by replacing dihydrate gypsum meets the standard of GB/T21371-2008 (industrial by-product gypsum used in cement) as a cement speed regulator.
Example 3
Sulfuric acid mother liquor wastewater of a certain Shandong factory, and raw water quality: COD was 3425mg/L, sulfuric acid content was 9.5%, TDS (total dissolved solids) was 143350mg/L.
The method for treating the wastewater containing sulfuric acid and sulfate comprises the following steps:
(1) Adding 27.5% (mass fraction) 1050mg/L hydrogen peroxide into chemical wastewater containing sulfuric acid and sulfate, and stirring for reacting for 1 hour;
(2) Adjusting the pH of the water treated in the step (1) to 5 by using calcium hydroxide;
(3) The water treated in the step (2) enters an ozone reactor for direct oxidation reaction for 1.5 hours, and the catalyst of the ozone oxidation reaction is SAO 3-II series high-efficiency ozone catalyst which is a commercial product;
(4) Adding alkali into the water treated in the step (3) to adjust the pH value to 9;
(5) The water treated in the step (4) enters an ozone reactor, and continues to carry out advanced ozone oxidation reaction for 1 hour, wherein the catalyst of the ozone oxidation reaction is SAO 3-II series high-efficiency ozone catalyst which is a commercially available product;
(6) And (4) respectively carrying out filter pressing, washing and drying on the water treated in the step (5) to obtain white crystals, namely the refined gypsum. Meanwhile, filter-pressing filtrate enters a normal sewage treatment system.
The final white crystals were taken for purity determination. The test is repeated three times, and the final white crystal is calcium sulfate crystal with average purity of more than 76%. Through cement tests, the type I portland cement prepared by replacing dihydrate gypsum meets the standard of GB/T21371-2008 (industrial by-product gypsum used in cement) as a cement speed regulator.
Example 4
The method takes the high-concentration sulfuric acid wastewater comprehensive water of a certain factory in Hebei as a treatment object, and the water quality of raw water is as follows: the total COD was 25580mg/L, the sulfuric acid content was 3.5%, the TDS (total dissolved solids) was 16800mg/L
The method for treating the wastewater containing sulfuric acid and sulfate comprises the following steps:
(1) Adding 27.5 percent (mass fraction) 18500mg/L hydrogen peroxide into chemical wastewater containing sulfuric acid and sulfate, and stirring for reaction for 1.5 hours;
(2) Adjusting the pH of the water treated in the step (1) to 4.5 by using calcium hydroxide;
(3) The water treated in the step (2) enters an ozone reactor for direct oxidation reaction for 2 hours, and the catalyst of the ozone oxidation reaction is SAO 3-II series high-efficiency ozone catalyst which is a commercial product;
(4) Adding alkali into the water treated in the step (3) to adjust the pH value to 8;
(5) The water treated in the step (4) enters an ozone reactor, and continues to carry out advanced ozone oxidation reaction for 1 hour, wherein the catalyst of the ozone oxidation reaction is SAO 3-II series high-efficiency ozone catalyst which is a commercially available product;
(6) And (4) respectively carrying out filter pressing, washing and drying on the water treated in the step (5) to obtain white crystals. Namely the refined gypsum. Meanwhile, filter-pressing filtrate enters a normal sewage treatment system.
The final white crystals were taken for purity determination. And repeating the test for three times, wherein the final white crystal is calcium sulfate crystal with average purity of more than 76%, and the calcium sulfate crystal is subjected to a cement test to replace I-type portland cement prepared from dihydrate gypsum, and meets the standard of GB/T21371-2008 (industrial by-product gypsum used in cement) as a cement speed regulator.
Example 5
The method takes the high-concentration sulfuric acid wastewater comprehensive water of a certain factory in Hebei as a treatment object, and the water quality of raw water is as follows: the total COD was 25580mg/L, the sulfuric acid content was 3.5%, the TDS (total dissolved solids) was 16800mg/L
The method for treating the wastewater containing sulfuric acid and sulfate comprises the following steps:
(1) Adding 27.5% (mass fraction) 18600mg/L hydrogen peroxide into chemical wastewater containing sulfuric acid and sulfate, and stirring for reaction for 1 hour;
(2) Adjusting the pH value of the water treated in the step (1) to 5 by using calcium hydroxide;
(3) the water treated in the step (2) enters an ozone reactor to carry out direct oxidation reaction for 2 hours, wherein the catalyst of the ozone oxidation reaction is SAO 3-II series high-efficiency ozone catalyst which is a commercially available product;
(4) Adding alkali into the water treated in the step (3) to adjust the pH value to 8;
(5) The water treated in the step (4) enters an ozone reactor, and continues to carry out advanced ozone oxidation reaction for 1 hour, wherein the catalyst of the ozone oxidation reaction is SAO 3-II series high-efficiency ozone catalyst which is a commercially available product;
(6) And (4) respectively carrying out filter pressing, washing and drying on the water treated in the step (5) to obtain white crystals. Namely the refined gypsum. Meanwhile, filter-pressing filtrate enters a normal sewage treatment system.
The final white crystals were taken for purity. And repeating the test for three times, wherein the final white crystal is calcium sulfate crystal with average purity of more than 76%, and the calcium sulfate crystal is subjected to a cement test to replace I-type portland cement prepared from dihydrate gypsum, and meets the standard of GB/T21371-2008 (industrial by-product gypsum used in cement) as a cement speed regulator.
Example 6
The comprehensive water of high-concentration sulfuric acid wastewater of a certain factory in Hebei is taken as a treatment object, and the water quality of raw water is as follows: the total COD was 25580mg/L, the sulfuric acid content was 3.5%, the TDS (total dissolved solids) was 16800mg/L
The method for treating the wastewater containing sulfuric acid and sulfate comprises the following steps:
(1) Adding 27.5 percent (mass fraction) 18600mg/L hydrogen peroxide into chemical wastewater containing sulfuric acid and sulfate, and stirring for reaction for 1 hour;
(2) Adjusting the pH of the water treated in the step (1) to 4 by using calcium hydroxide;
(3) The water treated in the step (2) enters an ozone reactor for direct oxidation reaction for 2 hours, and the catalyst of the ozone oxidation reaction is SAO 3-II series high-efficiency ozone catalyst which is a commercial product;
(4) Adding alkali into the water treated in the step (3) to adjust the pH value to 9;
(5) The water treated in the step (4) enters an ozone reactor, and continues to carry out advanced ozone oxidation reaction for 0.5 hour, wherein the catalyst of the ozone oxidation reaction is SAO 3-II series high-efficiency ozone catalyst which is a commercial product;
(6) And (4) respectively carrying out filter pressing, washing and drying on the water treated in the step (5) to obtain white crystals. Namely the refined gypsum. Meanwhile, filter-pressing filtrate enters a normal sewage treatment system.
The final white crystals were taken for purity determination. And repeating the test for three times, wherein the final white crystal is calcium sulfate crystal with the average purity of more than 76 percent, and the calcium sulfate crystal is subjected to a cement test to replace I-type portland cement prepared by dihydrate gypsum, thereby meeting the standard of GB/T21371-2008 (industrial by-product gypsum used in cement) as a cement speed regulator.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and amendments can be made without departing from the principle of the present invention, and these modifications and amendments should also be considered as the protection scope of the present invention.
Claims (10)
1. A method for refining gypsum from chemical wastewater containing sulfuric acid and sulfate comprises the following steps:
(1) Adding hydrogen peroxide into chemical wastewater containing sulfuric acid and sulfate, and stirring for reaction;
(2) Adjusting the pH of the water treated in the step (1) to 4-5 by using calcium hydroxide;
(3) the water treated in the step (2) enters an ozone reactor to carry out ozone oxidation reaction;
(4) Adding alkali into the water treated in the step (3) to adjust the pH value to 8-9;
(5) The water treated in the step (4) enters an ozone reactor, and the ozone oxidation reaction is continuously carried out;
(6) And (4) respectively carrying out filter pressing, washing and drying on the water treated in the step (5) to obtain white crystals, namely the refined gypsum.
2. The method for refining gypsum from chemical wastewater containing sulfuric acid and sulfates according to claim 1,
the concentration of sulfuric acid in the chemical wastewater containing sulfuric acid and sulfate in the step (1) is 2-10%.
3. The method for refining gypsum from chemical wastewater containing sulfuric acid and sulfates according to claim 1,
in the step (1), the concentration of hydrogen peroxide is 27.5%;
the adding amount of the hydrogen peroxide in the step (1) is 10-50% of the weight of COD in the chemical wastewater containing sulfuric acid and sulfate.
4. The method for refining gypsum from chemical wastewater containing sulfuric acid and sulfates according to claim 1, wherein the stirring reaction time in step (1) is 1h to 2h.
5. The method for refining gypsum from chemical wastewater containing sulfuric acid and sulfates according to claim 1,
and (3) suspending the calcium hydroxide in 30% in the step (2).
6. The method for refining gypsum from chemical wastewater containing sulfuric acid and sulfates according to claim 1,
the catalyst for the ozone oxidation reaction in the step (3) is an SAO 3-II series high-efficiency ozone catalyst.
7. The method for refining gypsum according to claim 1, wherein the ozone oxidation reaction time in step (3) is 1-2h.
8. The method for refining gypsum from chemical wastewater containing sulfuric acid and sulfates according to claim 1,
and (4) the alkali is 30% calcium hydroxide suspension.
9. The method for refining gypsum from chemical wastewater containing sulfuric acid and sulfates according to claim 1,
the catalyst for the ozone oxidation reaction in the step (5) is an SAO 3-II series high-efficiency ozone catalyst.
10. The method for refining gypsum from chemical wastewater containing sulfuric acid and sulfates according to claim 1, wherein the ozone oxidation reaction time of step (5) is 0.5 to 1 hour.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4344925A (en) * | 1979-01-12 | 1982-08-17 | Societe Chimique Des Charbonnages | Ozone whitening of synthetic gypsum |
| JP2018168024A (en) * | 2017-03-30 | 2018-11-01 | 住友大阪セメント株式会社 | Production method of plaster, and production method of cement composition |
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- 2022-10-21 CN CN202211297380.0A patent/CN115504499A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4344925A (en) * | 1979-01-12 | 1982-08-17 | Societe Chimique Des Charbonnages | Ozone whitening of synthetic gypsum |
| JP2018168024A (en) * | 2017-03-30 | 2018-11-01 | 住友大阪セメント株式会社 | Production method of plaster, and production method of cement composition |
Non-Patent Citations (1)
| Title |
|---|
| 梁吉艳等: "《环境工程学》", vol. 1, 中国建材工业出版社, pages: 67 * |
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