CN112028094A - Method for preparing magnesium hydroxide and calcium chloride by treating desulfurization wastewater of coal-fired power plant - Google Patents
Method for preparing magnesium hydroxide and calcium chloride by treating desulfurization wastewater of coal-fired power plant Download PDFInfo
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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
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
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- 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
- C01F11/20—Halides
- C01F11/24—Chlorides
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- 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
- C01F11/20—Halides
- C01F11/24—Chlorides
- C01F11/30—Concentrating; Dehydrating; Preventing the adsorption of moisture or caking
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- 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
- C01F11/20—Halides
- C01F11/24—Chlorides
- C01F11/32—Purification
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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
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
- C01F5/145—Purification
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- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
- C01F5/22—Magnesium hydroxide from magnesium compounds with alkali hydroxides or alkaline- earth oxides or hydroxides
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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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/101—Sulfur compounds
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/18—Nature of the water, waste water, sewage or sludge to be treated from the purification of gaseous effluents
Abstract
A method for preparing magnesium hydroxide and calcium chloride by treating desulfurization wastewater of a coal-fired power plant comprises the following steps: step 1, neutralization pretreatment; step 2, reacting and synthesizing magnesium hydroxide; step 3, press-filtering, washing and drying magnesium hydroxide; and 4, drying the calcium chloride. Aiming at the characteristic that the concentration of magnesium, calcium, sulfate radicals and chloride ions in the desulfurization concentrated wastewater of the coal-fired power plant is higher, slaked lime is added into the desulfurization concentrated wastewater for neutralization pretreatment, impurities such as sulfate radicals and heavy metals are removed, then magnesium hydroxide and calcium chloride are synthesized by utilizing the chemical reaction of magnesium ions and lime milk, finally separation and drying are carried out, and the magnesium hydroxide solid and the calcium chloride solid are recovered, so that the resource recovery of the wastewater is realized while the problem of wastewater pollution is solved.
Description
Technical Field
The invention relates to the field of wastewater treatment, and particularly belongs to a method for preparing magnesium hydroxide and calcium chloride by treating desulfurization wastewater of a coal-fired power plant.
Background
The wide application of the limestone wet desulphurization technology in coal-fired power plants leads to the increasing production of the by-product of wet desulphurization, namely desulphurization waste water, and the aim of discharging the desulphurization waste water is to discharge elements such as chloride ions enriched in the treatment process and prevent the stable operation of the system from being damaged by overhigh ion concentration. At present, domestic and overseas research mainly focuses on the treatment technology of the desulfurization wastewater, and due to the consideration of factors such as cost, market and the like, the attention of the desulfurization wastewater recycling technology is gradually weakened. However, a large number of elements in the desulfurization wastewater are potential resources, and the ions such as chlorine, magnesium and calcium are removed and separated, so that zero emission of the desulfurization wastewater can be realized, the aim of recycling salts is fulfilled, and the method can be used as a technical reserve for zero emission of the desulfurization wastewater.
The pH value of the desulfurization waste water concentrated solution is about 1, and the desulfurization waste water concentrated solution contains a large amount of chloride ions and magnesium ions, and the composition characteristics of the desulfurization waste water concentrated solution are close to those of bittern, so that the preparation of magnesium hydroxide and calcium chloride by using a bittern salt preparation technology can be referred. However, the desulfurization waste water contains a large amount of impurities, such as sulfate radicals, carbonate radicals, heavy metals and the like, and the removal process is complex, which affects the purity of magnesium hydroxide.
Disclosure of Invention
The invention aims to provide a method for preparing magnesium hydroxide and calcium chloride by treating desulfurization wastewater of a coal-fired power plant, and aims to solve the technical problems of high cost, complex impurity removal and product separation process, low product purity and the like of the conventional desulfurization wastewater treatment technology.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing magnesium hydroxide and calcium chloride by treating desulfurization wastewater of a coal-fired power plant is characterized by comprising the following steps:
step 1, neutralization pretreatment: adding a neutralizing agent into the desulfurization concentrated wastewater, controlling the pH value to be 8.0-9.0, and removing suspended matters, heavy metals and calcium sulfate from the neutralized mixed solution through solid-liquid separation to obtain supernatant containing Mg2+、Ca2+、Cl-Ions, analyzing and recording the concentration of each ion, mainly carrying out the following chemical reactions,
2OH-+M2+→M(OH)2↓
wherein M is2+Is a heavy metal ion;
step 2, magnesium hydroxide reaction synthesis: preparing acidified water, and preparing 2mol/L lime milk by using the acidified water and slaked lime; adding deionized water into a container in advance, simultaneously adding the supernatant and lime milk into ionized water for mixing, determining flow of the supernatant and the lime milk according to the content of magnesium ions in the supernatant, and controlling the feeding molar ratio Ca (OH)2:Mg2+Controlling pH value to 10.0-11.0 at 1:1 to produce magnesium hydroxide suspension, mainly carrying out the following chemical reactions,
Ca(OH)2+Mg2+→Mg(OH)2↓+Ca2+
step 3, pressure filtration, washing and drying of magnesium hydroxide: filtering and separating the magnesium hydroxide suspension to obtain magnesium hydroxide solid and filtrate, filtering and washing the magnesium hydroxide solid, drying to obtain a magnesium hydroxide product, and simultaneously collecting the filtrate and washing liquid to mix into a calcium chloride solution;
step 4, drying calcium chloride: the calcium chloride solution is subjected to membrane concentration, and concentrated water is dried and crystallized to generate CaCl2·2H2And O, recycling the obtained fresh water to the step 2 for preparing acidified water, and treating the desulfurization wastewater of the coal-fired power plant to prepare magnesium hydroxide and calcium chloride.
Further preferably, the method for preparing acidified water in step 2 is to add concentrated hydrochloric acid into fresh water to remove carbonate, then aerate for 30min to remove carbon dioxide, and control pH at 3-3.5, mainly to perform the following chemical reactions,
further, the neutralizing agent in the step 1 is slaked lime, the feeding speed is 1g/min, the stirring is carried out for 30min, the rotating speed is 200rpm, and the solid-liquid separation method is filtering through a plate-and-frame filter press.
In addition, the acidified water and the slaked lime in the step 2 are mixed and stirred for 30-35 min to form lime milk, an overflow port is formed in the container, the feeding and staying time of the supernatant and the lime milk is 6.5-7 h, and the stirring speed is 100 rpm.
More preferably, the washing liquid for washing in the step 3 is acidified water
Compared with the prior art, the invention has the following characteristics and beneficial effects:
aiming at the characteristic that the concentration of magnesium, calcium, sulfate radicals and chloride ions in the desulfurization concentrated wastewater of the coal-fired power plant is higher, slaked lime is added into the desulfurization concentrated wastewater for neutralization pretreatment, impurities such as sulfate radicals and heavy metals are removed, then magnesium hydroxide and calcium chloride are synthesized by utilizing the chemical reaction of magnesium ions and lime milk, finally separation and drying are carried out, and the magnesium hydroxide solid and the calcium chloride solid are recovered, so that the resource recovery of the wastewater is realized while the problem of wastewater pollution is solved.
The invention uses a small amount of medicaments, only needs concentrated hydrochloric acid and slaked lime, does not introduce other ions, and does not need to add seed crystals, flocculating agents and dispersing agents; the removal rate of carbonate and sulfate radicals is high, and the magnesium hydroxide is a nano-grade product and has high purity and commercial value; the method has the advantages of utilizing the heat source advantages of the coal-fired power plant, reducing the drying cost of calcium chloride, synchronously separating and recycling calcium and magnesium, having short process flow, simple operation, easy realization of automatic control, low cost, simple process and convenient control, being an important direction for researching zero emission of desulfurization wastewater, and having great significance for improving the environmental protection technical level of the coal-fired power plant and promoting the circular economy.
Drawings
FIG. 1 is a flow chart of a method for preparing magnesium hydroxide and calcium chloride by treating desulfurization wastewater of a coal-fired power plant according to the present invention.
Detailed Description
In order to make the technical means, innovative features, objectives and functions realized by the present invention easy to understand, the present invention is further described below.
The examples described herein are specific embodiments of the present invention, are intended to be illustrative and exemplary in nature, and are not to be construed as limiting the scope of the invention. In addition to the embodiments described herein, those skilled in the art will be able to employ other technical solutions which are obvious based on the disclosure of the claims and the specification of the present application, and these technical solutions include technical solutions which make any obvious replacement or modification for the embodiments described herein.
A method for preparing magnesium hydroxide and calcium chloride by treating desulfurization wastewater of a coal-fired power plant is shown in figure 1 and comprises the following steps:
step 1, neutralization pretreatment: adding a neutralizer into the desulfurization concentrated wastewater, wherein the neutralizer is slaked lime, the feeding speed is 1g/min, stirring is carried out for 30min, the rotating speed is 200rpm, and the solid-liquid separation method comprises filtering by a plate-and-frame filter pressThe pH value is controlled to be 8.0-9.0 to generate the CaSO with good sedimentation performance and in the shape of conglutinated crystal cluster4Precipitating, neutralizing, removing suspended matters, heavy metals and calcium sulfate from the mixed solution through solid-liquid separation to obtain supernatant containing Mg2+、Ca2+、Cl-Ions, analyzing and recording the concentration of each ion to provide conditions for the subsequent preparation of high-purity magnesium hydroxide, wherein the following chemical reactions mainly occur in the step,
2OH-+M2+→M(OH)2↓
wherein M is2+Is a heavy metal ion;
step 2, magnesium hydroxide reaction synthesis: preparing acidified water by adding concentrated hydrochloric acid into fresh water to remove carbonate, aerating for 30min to remove carbon dioxide, controlling pH at 3-3.5, mainly performing the following chemical reactions,
mixing acidified water and slaked lime, stirring for 30-35 min to form lime milk, and preparing to form 2mol/L lime milk; adding deionized water into a container in advance, simultaneously adding the supernatant and the lime cream into ionized water for mixing, wherein the feeding residence time of the supernatant and the lime cream is 6.5-7 h, the stirring speed is 100rpm, an overflow port is arranged on the container, the flow rate of the supernatant and the lime cream is determined according to the content of magnesium ions in the supernatant, and the feeding molar ratio Ca (OH) is controlled2:Mg2+Controlling pH value to 10.0-11.0 at 1:1 to produce magnesium hydroxide suspension, mainly carrying out the following chemical reactions,
Ca(OH)2+Mg2+→Mg(OH)2↓+Ca2+
step 3, pressure filtration, washing and drying of magnesium hydroxide: filtering and separating the magnesium hydroxide suspension to obtain magnesium hydroxide solid and filtrate, washing the magnesium hydroxide solid, selecting the acidified water prepared in the step 2 as washing liquid, filtering after washing, circulating for 3 times, filtering and washing the magnesium hydroxide solid, drying to obtain a magnesium hydroxide product, and simultaneously collecting the filtrate and the washing liquid to be mixed into calcium chloride solution;
step 4, drying calcium chloride: the calcium chloride solution is subjected to membrane concentration, and concentrated water is dried and crystallized to generate CaCl2·2H2And O, recycling the obtained fresh water to the step 2 for preparing acidified water, and treating the desulfurization wastewater of the coal-fired power plant to prepare magnesium hydroxide and calcium chloride.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. A method for preparing magnesium hydroxide and calcium chloride by treating desulfurization wastewater of a coal-fired power plant is characterized by comprising the following steps:
step 1, neutralization pretreatment: adding a neutralizing agent into the desulfurization concentrated wastewater, controlling the pH value to be 8.0-9.0, and removing suspended matters, heavy metals and calcium sulfate from the neutralized mixed solution through solid-liquid separation to obtain supernatant containing Mg2+、Ca2+、Cl-Ions, analyzing and recording the concentration of each ion, mainly carrying out the following chemical reactions,
2OH-+M2+→M(OH)2↓
wherein M is2+Is a heavy metal ion;
step 2, magnesium hydroxide reaction synthesis: preparing acidified water, and preparing 2mol/L lime milk by using the acidified water and slaked lime; adding deionized water into a container in advance, simultaneously adding the supernatant and lime milk into ionized water for mixing, determining flow of the supernatant and the lime milk according to the content of magnesium ions in the supernatant, and controlling the feeding molar ratio Ca (OH)2:Mg2+＝1:1，pH value is controlled to be 10.0-11.0, magnesium hydroxide suspension is generated, the following chemical reactions mainly occur,
Ca(OH)2+Mg2+→Mg(OH)2↓+Ca2+
step 3, pressure filtration, washing and drying of magnesium hydroxide: filtering and separating the magnesium hydroxide suspension to obtain magnesium hydroxide solid and filtrate, filtering and washing the magnesium hydroxide solid, drying to obtain a magnesium hydroxide product, and simultaneously collecting the filtrate and washing liquid to mix into a calcium chloride solution;
step 4, drying calcium chloride: the calcium chloride solution is subjected to membrane concentration, and concentrated water is dried and crystallized to generate CaCl2·2H2And O, recycling the obtained fresh water to the step 2 for preparing acidified water, and treating the desulfurization wastewater of the coal-fired power plant to prepare magnesium hydroxide and calcium chloride.
2. The method for preparing magnesium hydroxide and calcium chloride by treating desulfurization wastewater of a coal-fired power plant according to claim 1, characterized in that: the method for preparing the acidified water in the step 2 is to add concentrated hydrochloric acid into fresh water to remove carbonate, then aerate for 30min to remove carbon dioxide, control the pH value to be 3-3.5, mainly carry out the following chemical reactions,
3. the method for preparing magnesium hydroxide and calcium chloride by treating desulfurization wastewater of a coal-fired power plant according to claim 1, characterized in that: the neutralizing agent in the step 1 is slaked lime, the feeding speed is 1g/min, the stirring is carried out for 30min, the rotating speed is 200rpm, and the solid-liquid separation method is filtering through a plate-and-frame filter press.
4. The method for preparing magnesium hydroxide and calcium chloride by treating desulfurization wastewater of a coal-fired power plant according to claim 1, characterized in that: and (3) mixing the acidified water and the slaked lime in the step (2), stirring for 30-35 min to form lime milk, arranging an overflow port on the container, and feeding the supernatant and the lime milk for 6.5-7 h at the stirring speed of 100 rpm.
5. The method for preparing magnesium hydroxide and calcium chloride by treating desulfurization wastewater of a coal-fired power plant according to claim 1, characterized in that: and the washing liquid for washing in the step 3 is acidified water.
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| CN202010711125.0A CN112028094A (en) | 2020-07-22 | 2020-07-22 | Method for preparing magnesium hydroxide and calcium chloride by treating desulfurization wastewater of coal-fired power plant |
| CN202011483586.3A CN112357939A (en) | 2020-07-22 | 2020-12-16 | Method for preparing magnesium hydroxide and calcium chloride by treating desulfurization wastewater of coal-fired power plant |
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| CN202011483586.3A Pending CN112357939A (en) | 2020-07-22 | 2020-12-16 | Method for preparing magnesium hydroxide and calcium chloride by treating desulfurization wastewater of coal-fired power plant |
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| CN113955893A (en) * | 2021-11-24 | 2022-01-21 | 内蒙古国华呼伦贝尔发电有限公司 | Desulfurization wastewater treatment method and system |
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| CN114602926A (en) * | 2022-03-07 | 2022-06-10 | 李晓清 | Device and process for resourceful treatment of waste incineration fly ash |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP1110595A1 (en) * | 1999-12-23 | 2001-06-27 | Dravo Lime, Inc. | Reduction of calcium and chloride in the flue gas desulfurization process |
| CN1415541A (en) * | 2002-12-16 | 2003-05-07 | 南风化工集团股份有限公司 | Technique for producing magnesium hydroxide, barium choride and sulfureted hydrogen from brine water in salt lake |
| CN103754901A (en) * | 2014-01-21 | 2014-04-30 | 江苏仁欣化工股份有限公司 | Method for producing magnesium hydroxide from mixed solution containing magnesium chloride and calcium chloride by lime seeding method |
| CN104261443A (en) * | 2014-09-25 | 2015-01-07 | 池州西恩新材料科技有限公司 | Process for calcium-method production of magnesium hydrate by using nanofiltration membrane |
| CN106492615B (en) * | 2016-11-08 | 2020-03-27 | 神华集团有限责任公司 | Desulfurization method and desulfurization system for coal-fired flue gas |
| CN107619137B (en) * | 2017-10-10 | 2020-07-14 | 华北电力大学（保定） | Method for recycling calcium and magnesium in desulfurization wastewater by carbonization method |
| CN109264761B (en) * | 2018-10-30 | 2022-02-11 | 华北电力大学（保定） | Method for recycling calcium and magnesium ions in desulfurization wastewater by lime milk method |
| CN109748422A (en) * | 2019-02-27 | 2019-05-14 | 华能沁北发电有限责任公司 | A kind of device and method recycling magnesium in high magnesium desulfurization wastewater |
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| CN113955893A (en) * | 2021-11-24 | 2022-01-21 | 内蒙古国华呼伦贝尔发电有限公司 | Desulfurization wastewater treatment method and system |
| CN113955893B (en) * | 2021-11-24 | 2023-08-22 | 内蒙古国华呼伦贝尔发电有限公司 | Desulfurization wastewater treatment method and treatment system |
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Application publication date: 20201204 |