CN113264541B - Magnesium removal method and device for crude brine - Google Patents

Magnesium removal method and device for crude brine Download PDF

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Publication number
CN113264541B
CN113264541B CN202110552604.7A CN202110552604A CN113264541B CN 113264541 B CN113264541 B CN 113264541B CN 202110552604 A CN202110552604 A CN 202110552604A CN 113264541 B CN113264541 B CN 113264541B
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settling agent
tank
brine
crude
magnesium
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CN113264541A (en
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孙在勇
马传阳
孙风春
王琳琳
张健
王晓波
潘学彬
王猛
孙中杰
杨兴海
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Shandong Haihua Co ltd
Shandong Haihua Group Co Ltd
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Shandong Haihua Co ltd
Shandong Haihua Group Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D3/00Halides of sodium, potassium or alkali metals in general
    • C01D3/14Purification
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
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Abstract

The invention discloses a method and a device for removing magnesium from crude brine, which comprises a chemical precipitation aid device, a salt dissolving barrel, a crude brine launder, a front labyrinth groove, a mixed solution concentration tank, a rear labyrinth groove, a parallel launder and a primary clarifying barrel which are sequentially connected through pipelines; the front curve groove is provided with a lime milk pipeline interface; the magnesium removal method comprises the steps that the reaction time of crude salt water and lime milk is controlled to be 30-50S, the temperature of the precipitation aid is controlled to be 40-45 ℃, the reflux ratio is 30% -40%, and a primary precipitation aid is added before the blending liquid enters a clarifying barrel. The invention can achieve the purposes of improving the magnesium removal effect of crude brine, reducing the internal scab of equipment, stabilizing the production working condition, reducing the consumption and improving the product quality.

Description

Method and device for removing magnesium from crude brine
Technical Field
The invention relates to a method and a device for removing magnesium from crude brine.
Background
In the ammonia-soda process for preparing alkali, the task of the brine refining process is to prepare qualified refined brine for subsequent production, and the original salt is dissolved to prepare the qualified refined brineThe brine is formed into high-concentration brine, namely crude brine, and the impurity water for dissolving salt comprises fresh water, seawater, brine sludge washing water and the like, so that in order to reduce calcium and magnesium ion impurities brought into a system, a nanofiltration refined brine technology is developed and applied in recent years, and the cost for subsequently refining brine can be greatly reduced by adopting nanofiltration refined brine; adding lime milk into the crude brine to remove magnesium in the crude brine to obtain primary brine; and removing calcium in the primary brine by using ammonia and carbon dioxide to obtain secondary brine, namely refined brine. The quality of the soda ash product is improved, water-insoluble magnesium carbonate, calcium carbonate and the like in the soda ash product mainly come from magnesium and calcium salts in the brine, and the purification of the brine can remove magnesium and calcium impurities, thereby being beneficial to the improvement of the quality of the soda ash product and enhancing the competitiveness of the product; secondly, the scabs inside the equipment and the pipeline in the subsequent production process are reduced, and the magnesium and calcium salts in the brine and CO in the subsequent production process2And NH3Reaction to form Mg (OH)2、CaCO3Precipitation and Mg CO3·Mg(OH)2·3H2O、NaCl·MgCO3·Na2CO3After the double salt is crystallized, scabbing is generated inside equipment and pipelines to cause blockage, so that the equipment capacity is reduced, and the operation period is greatly shortened; and thirdly, the loss of ammonia, sodium chloride and carbon dioxide in the production process is reduced, and magnesium and calcium impurities in the brine are removed in the subsequent process, so that the loss of ammonia, sodium chloride and carbon dioxide is caused, and the utilization rate of raw materials is reduced.
There are generally four methods for brine refining, namely, lime-soda process, lime-ammonium carbonate process, and lime-mirabilite process. The old line of Shandong sea soda plant adopts a brine refining process by a lime-ammonium carbonate method, namely, lime milk, ammonia and carbon dioxide are utilized to remove magnesium and calcium salt in crude brine, and the magnesium and calcium removal of the crude brine is carried out in two steps. Firstly, adding ash (the ash refers to lime milk) into crude brine to remove magnesium, wherein the chemical reaction comprises the following steps:
Mg2+ + Ca(OH)2 → Mg(OH)2 + Ca2+
the clear liquid after magnesium removal, namely primary brine enters a calcium removal tower to react with carbonated tail gas, and Ca is generated by the magnesium removal reaction2+And Ca inherent in crude brine2+Calcium carbonate precipitate is generated and removed, and the chemical reaction for removing calcium is as follows:
NH3 + H2O + CO2 → (NH4)2CO3
Ca2+ + (NH4)2CO3 →CaCO3 + 2NH4 +
the process requirements of the primary brine obtained after the ash is added into the crude brine and the magnesium is removed meet two requirements in quality, wherein firstly, magnesium ions must be completely precipitated in the primary brine, secondly, the turbidity of the primary brine must be controlled below 150ppm, and otherwise, the magnesium ions remained in the primary brine and the magnesium hydroxide carried in the primary brine are precipitated to become magnesium ions in refined brine and enter a subsequent production system, thereby causing great difficulty in production.
The conventional crude brine magnesium removal apparatus generally comprises: the device comprises a dissolving and settling agent dissolving device, a salt dissolving barrel, a crude salt water flow groove, a mixed solution concentration groove, a labyrinth groove, a parallel flow groove and a primary clarifying barrel which are sequentially connected through pipelines, wherein the dissolving and settling agent dissolving device comprises a settling agent tank, a settling agent pump and a settling agent elevated tank which are sequentially connected, the mixed solution concentration groove is also connected with a lime milk pipeline, and the settling agent elevated tank is connected to the mixed solution concentration groove behind the lime milk pipeline. The process flow comprises the following steps: the crude salt water from the salt dissolving barrel passes through a mixed liquid collecting tank, a labyrinth tank, a parallel flow tank and a primary clarifying barrel in sequence through a crude salt water flow tank, the mixed liquid collecting tank is added with the lime milk through a lime milk pipeline, then the settling agent solution is added through a settling agent elevated tank, and finally the primary salt water and the primary sludge are obtained through the primary clarifying barrel. The solution of the crude brine mixed with the lime milk is called a blend.
The traditional crude brine magnesium removal device has the following problems:
1. the reaction time of the crude brine and the lime cream is insufficient, the mixing is not uniform, and the magnesium removal reaction is not complete.
The crude brine and the lime cream must have sufficient reaction time and be mixed uniformly to ensure complete magnesium removal reaction. In the device, the magnesium removal reaction is carried out in the mixed liquid concentration tank, the retention time of the crude brine and the lime milk in the concentration tank is short, the concentration tank is not stirred, the reaction time of the crude brine and the lime milk is insufficient, the mixing is not uniform, the magnesium removal reaction is not thorough, and magnesium ions which do not generate precipitates enter the subsequent process, so that the scab in the equipment is easily caused and the product quality is influenced. Before that, some manufacturers adopt a mixing liquid tank with stirring to carry out magnesium removal reaction, coarse brine and lime milk firstly enter the mixing liquid tank, are fully mixed and stay for a period of time and then enter a primary clarifying barrel, so that the magnesium removal reaction is completely reacted in the mixing liquid tank, but the mixing liquid tank has the problems of serious scabbing and difficult cleaning in the tank, and the yield of primary brine is seriously influenced. If change the mixing fluid tank into the concentrated groove of mixing fluid, compare with the mixing fluid tank, the clearance degree of difficulty and the frequency greatly reduced of the concentrated groove scab of mixing fluid, but corresponding again can cause the reaction time to shorten greatly, lead to except that the magnesium reaction is incomplete.
2. The temperature of the primary brine in winter is low, and the dissolution speed of polyacrylamide is slow.
The temperature of the water for the precipitation aid is required to be controlled within 60 ℃ and exceeds 60 ℃, so that the molecular weight of polyacrylamide is reduced, the precipitation aid effect is influenced, and the lower the water temperature is, the slower the dissolution speed of the polyacrylamide is, and the poorer the dissolution effect is. At present, the primary saline water precipitation aid is adopted, the temperature of primary saline water is only about 30 ℃ in winter, so that the polyacrylamide dissolution effect is poor, the dissolution is not easy to occur, pimples are easy to generate in a solvent, and the precipitation aid effect is influenced.
3. The mixing amount of the settling agent is adjusted lagged.
The flow meter is lacked on the liquid outlet pipeline of the settling agent head tank, and the flow of the settling agent must be judged by an operator according to the change of the liquid level of the head tank. When the production condition changes, the mixing amount of the settling agent is adjusted to be lagged, and the accurate control cannot be realized.
4. The path of the blending liquid is long, and the large magnesium hydroxide flocs are easy to be broken up in the flowing process.
The mixed liquid sequentially passes through a concentration tank, a labyrinth tank and a parallel flow tank and finally enters a primary clarifying barrel, and part of flocculated magnesium hydroxide precipitate is broken by impact in the flowing process, so that large flocs become broken, and the clarifying and settling effects are influenced.
The effect of magnesium removal of crude brine not only relates to the quality of the soda ash product, but also influences the stability of the production working condition and the level of production consumption. Particularly, in winter production, the temperature of the salt solution impurity water is gradually reduced along with the reduction of the air temperature, so that the sedimentation speed of magnesium hydroxide sediment in a clarifying barrel is reduced, the turbidity of primary brine is increased, magnesium ions which are not removed enter a subsequent production process to cause scabbing inside equipment and pipelines, the operation period of the equipment is shortened, the production working condition of subsequent production, particularly heavy sodium carbonate, is greatly influenced, the product quality is reduced, the consumption is increased, and even the quality accidents of turbid high-order product alkali occur.
Disclosure of Invention
The invention aims to provide a method and a device for removing magnesium from crude brine, which improve the precipitation assisting effect of a precipitation assisting agent and improve the clarification and separation efficiency of magnesium hydroxide precipitate, thereby achieving the purposes of reducing the turbidity of primary brine, improving the production working condition of soda ash and reducing the production consumption.
The method comprises a salt dissolving barrel, a crude salt water trough, a front labyrinth trough, a mixed solution concentration trough, a rear labyrinth trough, a parallel trough and a primary clarifying barrel which are sequentially connected through pipelines, and comprises the following steps:
(1) feeding the refined brine and the polyacrylamide into a settling agent tank, and stirring to fully dissolve the polyacrylamide to obtain a settling agent solution with the mass concentration of 0.8-1.0 thousandth (mass percentage);
(2) pumping the settling agent solution obtained in the step (1) to a settling agent elevated tank through a settling agent pump, wherein the settling agent elevated tank adopts high liquid level reflux operation, so that part of the settling agent solution flows back to a settling agent tank through an overflow pipeline, and the reflux ratio is controlled to be 30-40%;
(3) meanwhile, raw salt and mixed water enter a salt dissolving barrel to be dissolved to prepare crude salt water, wherein the salt content of the crude salt water is controlled to be 108-108.5 ti;
(4) the crude salt water prepared in the step (3) enters a front curve groove through a crude salt water groove, lime milk with the concentration of 150-160 ti is added and fully mixed with the crude salt water for magnesium removal reaction, and the flow of the lime milk is controlled to be 15-20m3H, coarseThe retention time of the salt water in the labyrinth groove is controlled to be 30-50s, and the surplus ash in the mixed liquid of the crude salt water and the lime cream is controlled to be 0.1-0.15 ti;
(5) allowing the mixed solution prepared in the step (4) to enter a mixed solution collecting tank, adding 0.8-1.0 per mill of settling agent solution obtained in the step (2), allowing the mixed solution to flow through a rear labyrinth tank for continuous flocculation, adding settling agent solution for further flocculation when the mixed solution flows through parallel flow tanks, and flocculating fine magnesium hydroxide suspended matters into large flocs; the flow of the settling agent solution from the elevated tank is controlled to be 8-9m3Respectively entering a mixed liquid concentration tank and a parallel flow tank;
(6) and (4) allowing the flocculated mixed solution prepared in the step (5) to enter a primary clarifying barrel for clarifying and settling treatment, controlling the retention time of the mixed solution in the primary clarifying barrel for 10-12 hours, and finally obtaining supernatant with turbidity of 80-100 ppm, removing calcium from the supernatant by a calcium removal tower through a primary brine pump, and removing mud from a mud washing barrel.
In the step (1), the temperature of refined salt water for dissolving the settling agent is controlled to be 40-45 ℃.
In order to solve the problem of incomplete magnesium removal reaction, a front curve groove is additionally arranged between a crude salt water flow groove and a mixed solution collecting groove, an ash emulsion pipeline is connected to the front curve groove, the retention time of crude salt water in the front curve groove is controlled to be 30-50S, the magnesium removal reaction time is prolonged, magnesium ions in the crude salt water are completely precipitated before entering a primary clarifying barrel, and compared with a mixed solution tank, the front curve groove has the advantages of large treatment capacity, capability of meeting the requirement of high-load production, easiness in scab cleaning and the like.
In order to improve the dissolution effect of polyacrylamide, refined salt water is used as the water for the chemical precipitation aid, the temperature of the water for the chemical precipitation aid is increased, the temperature of the refined salt water is controlled to be 40-45 ℃ in winter, and is increased by 10 ℃ compared with primary salt water, and the dissolution speed of the polyacrylamide can be remarkably increased by adopting the refined salt hydration precipitation aid.
The crude brine magnesium removal device for realizing the method comprises a chemical precipitation aid device, a salt dissolving barrel, a crude brine launder, a front curve groove, a mixed liquid concentration groove, a rear curve groove, a parallel launder and a primary clarifying barrel which are connected in sequence through pipelines; the front curve groove is provided with an ash emulsion pipeline interface; the settling agent dissolving device comprises a settling agent tank, a settling agent pump and a settling agent head tank which are sequentially connected, wherein the settling agent tank is provided with a stirring function and is provided with a settling agent feeding port and a refined brine feeding port, a liquid outlet pipeline of the settling agent head tank is divided into two paths, one path is connected to the mixed liquid concentration tank, and the other path is divided into two paths which are respectively connected to the settling agent solution feeding ports of the parallel flow tanks.
And a flowmeter is arranged on the liquid outlet pipeline of the settling agent elevated tank.
The settling agent elevated tank is provided with an overflow return pipeline connected to the settling agent tank.
The settling agent elevated tank adopts high liquid level reflux operation, so that part of settling agent solution flows back to the settling agent tank through an overflow pipeline, the dissolving effect of polyacrylamide is further improved, and the concentration of the settling agent solution is increased.
In order to solve the problem that large magnesium hydroxide flocs are broken up by impact in the flowing process, a settling agent adding point is added at each parallel flow groove of a primary clarifying barrel after a mixed solution collecting groove, and the settling agents are added in three points, so that the settling agents and the mixed solution can be uniformly mixed, the flocculation effect of magnesium hydroxide precipitation can be guaranteed, and the speed of clarifying and separating the magnesium hydroxide in the primary clarifying barrel can be improved.
By adding the flow meter on the liquid outlet pipeline of the settling agent elevated tank, the change of the flow of the settling agent can be monitored in real time, and the problem can be found and adjusted in time; and the device also can provide data reference for an operator when adjusting the flow of the settling agent, so as to achieve accurate control.
Drawings
The invention is further illustrated with reference to the following figures and examples:
fig. 1 is a schematic structural view of the present invention.
In the figure: 1. the system comprises a salt dissolving barrel, 2 parts of a crude salt solution tank, 3 parts of a front curve groove, 3 parts of a lime milk inlet, 4 parts of a mixed solution concentration tank, 4 parts of 1 part of a settling agent solution inlet, 5 parts of a rear curve groove, 6 parts of a first parallel tank, 6 parts of 1 part of a first settling agent solution inlet, 7 parts of a second parallel tank, 7 parts of 1 part of a second settling agent solution inlet, 8 parts of a primary clarifying barrel, 9 parts of a primary salt pump, 10 parts of a settling agent tank, 10 parts of 1 part of a polyacrylamide inlet, 10 parts of 2 parts of a fine salt solution inlet, 11 parts of a settling agent pump, 12 parts of a settling agent elevated tank, 13 parts of a settling agent overflow pipe, 14 parts of a flow meter.
Detailed Description
Example 1
Referring to fig. 1, the method for removing magnesium from crude brine comprises the following steps:
(1) feeding refined brine and polyacrylamide into a settling agent tank 10, controlling the temperature of the refined brine at 45 ℃, and fully dissolving the polyacrylamide by stirring to obtain a settling agent solution with the concentration of 0.8 per mill (mass percentage, the same below);
(2) conveying the settling agent solution obtained in the step (1) to a settling agent head tank 12 through a settling agent pump 11, wherein the settling agent head tank 12 adopts high liquid level reflux operation, so that part of the settling agent solution flows back to a settling agent tank 10 through an overflow pipeline 13, and the reflux ratio is controlled to be 40%;
(3) raw salt and mixed water enter a salt dissolving barrel 1, crude salt water is prepared by dissolution, and the salt content of the crude salt water is controlled to be 108 ti;
(4) the crude salt water prepared in the step (3) enters a front curve groove 3 through a crude salt water groove 2, lime milk with the concentration of 150ti is added and fully mixed with the crude salt water for magnesium removal reaction, and the flow of the lime milk is controlled to be 15m3The residence time of the crude brine in the labyrinth groove 3 is controlled to be 30S, and the surplus ash in the mixed liquid of the crude brine and the lime milk is controlled to be 0.1 ti;
(5) the mixed liquid prepared in the step (4) enters a mixed liquid collecting tank 4, 0.8 per mill of settling agent solution is added for flocculation, settling agent solution is added into a first parallel launder 6 and a second parallel launder 7 for further flocculation, and tiny magnesium hydroxide suspended matters are flocculated into large floccules through flocculation; the flow of the settling agent solution from the elevated tank is controlled to be 8.5m3Respectively entering a mixed liquid concentration tank and a parallel flow tank;
(6) and (3) allowing the flocculated mixed solution prepared in the step (5) to enter a primary clarifying barrel 8 for clarifying and settling treatment, controlling the retention time of the mixed solution in the primary clarifying barrel 8 for 10 hours to finally obtain supernatant with turbidity of 85ppm, conveying the supernatant to a calcium removal tower through a primary brine pump 9 to remove calcium, and removing primary mud from a mud washing barrel to wash mud.
The equipment adopted by the invention is universal equipment. ti refers to the titer, i.e., one twentieth of the equivalent concentration, which is used in the soda industry to express solution concentration.
By adopting the technical scheme of the invention, the dissolving speed of polyacrylamide can be increased, and the clarification and separation effects of magnesium hydroxide can be improved. Table 1 shows the comparison between the determination effect of example 1 of the present invention and the conventional apparatus, and the changes in the dissolution effect of the settling agent, the magnesium content of the crude brine, the turbidity of the supernatant of the blending solution, the turbidity of the primary brine, the turbidity of the refined brine, the yield of heavy sodium carbonate, and the turbidity of high-quality sodium carbonate are mainly observed, and the external operating conditions during the determination process are completely the same as those before the modification.
Table 1: example 1 comparison with conventional crude brine demagging apparatus operating data
Figure 713574DEST_PATH_IMAGE002
From the data comparison condition, the data of the invention is obviously better than the traditional device, and mainly shows that:
1) the dissolving effect of polyacrylamide is better than that of the traditional device, the concentration is increased by 0.06 thousandth, the temperature of the settling agent solution is increased by 9.4 ℃, and the 'pimple' in the settling agent solution completely disappears;
2) the turbidity of the supernatant of the mixed solution is reduced from 162ppm to 85ppm, and the transparency is good;
3) the turbidity of the primary brine is reduced by about 20ppm, and the turbidity of the refined brine is reduced by about 10 ppm;
4) the production of heavy sodium carbonate is increased by 100 tons, and the working condition of the heavy sodium carbonate is obviously improved;
5) the quality accident of the high-turbidity defective products does not occur.
The comparison shows that the invention achieves the purposes of improving the magnesium removal effect of the crude brine, reducing the scab in the equipment, stabilizing the production working condition, reducing the production consumption and improving the product quality.
Example 2
Referring to fig. 1, the magnesium removal method of crude brine comprises the following steps:
(1) feeding refined brine and polyacrylamide into a settling agent tank 10, controlling the temperature of the refined brine at 40 ℃, and fully dissolving the polyacrylamide by stirring to obtain a settling agent solution with the concentration of 1.0 per mill;
(2) conveying the settling agent solution obtained in the step (1) to a settling agent elevated tank 12 through a settling agent pump 11, wherein the settling agent elevated tank 12 adopts high liquid level reflux operation to enable part of the settling agent solution to flow back to a settling agent tank 10 through an overflow pipeline 13, and the reflux ratio is controlled to be 30%;
(3) raw salt and mixed water enter a salt dissolving barrel 1, crude salt water is prepared by dissolution, and the salt content of the crude salt water is controlled to be 108.5 ti;
(4) the crude salt water prepared in the step (3) enters a front curve groove 3 through a crude salt water groove 2, lime milk with the concentration of 160ti is added and fully mixed with the crude salt water for magnesium removal reaction, and the flow of the lime milk is controlled to be 20m3The residence time of the crude brine in the labyrinth groove 3 is controlled to be 50S, and the surplus ash in the mixed liquid of the crude brine and the lime milk is controlled to be 0.15 ti;
(5) the mixed liquid prepared in the step (4) enters a mixed liquid collecting tank 4, 1.0 per mill of settling agent solution is added for flocculation, settling agent solution is added into a first parallel launder 6 and a second parallel launder 7 for further flocculation, and tiny magnesium hydroxide suspended matters are flocculated into large floccules through flocculation; the flow of the settling agent solution from the elevated tank is controlled to be 8m3Respectively entering a mixed liquid centralized tank and a parallel flow tank;
(6) and (3) allowing the flocculated mixed solution prepared in the step (5) to enter a primary clarifying barrel 8 for clarifying and settling treatment, controlling the retention time of the mixed solution in the primary clarifying barrel 8 for 12 hours to finally obtain supernatant with turbidity of 80ppm, conveying the supernatant to a calcium removal tower through a primary brine pump 9 to remove calcium, and removing primary mud from a mud washing barrel to wash mud.
Table 2: example 2 compares the data with the conventional crude brine magnesium removal plant operation.
Figure 693031DEST_PATH_IMAGE003
Example 3
Referring to fig. 1, a method for removing magnesium from crude brine includes the following steps:
(1) feeding refined brine and polyacrylamide into a settling agent tank 10, controlling the temperature of the refined brine at 42 ℃, and fully dissolving the polyacrylamide by stirring to obtain a settling agent solution with the concentration of 0.9 per mill;
(2) conveying the settling agent solution obtained in the step (1) to a settling agent elevated tank 12 through a settling agent pump 11, wherein the settling agent elevated tank 12 adopts high liquid level reflux operation to enable part of the settling agent solution to flow back to a settling agent tank 10 through an overflow pipeline 13, and the reflux ratio is controlled to be 35%;
(3) raw salt and mixed water enter a salt dissolving barrel 1, crude salt water is prepared by dissolution, and the salt content of the crude salt water is controlled to be 108 ti;
(4) the crude salt water prepared in the step (3) enters a front curve groove 3 through a crude salt water launder 2, lime milk with the concentration of 155ti is added to be fully mixed with the crude salt water for magnesium removal reaction, and the flow of the lime milk is controlled to be 18m3The residence time of the crude brine in the labyrinth groove 3 is controlled to be 40S, and the surplus ash in the mixed liquid of the crude brine and the lime milk is controlled to be 0.12 ti;
(5) the mixed liquid prepared in the step (4) enters a mixed liquid collecting tank 4, 0.9 per mill of settling agent solution is added for flocculation, settling agent solution is added into a first parallel launder 6 and a second parallel launder 7 for further flocculation, and tiny magnesium hydroxide suspended matters are flocculated into large floccules through flocculation; flow rate of settling agent solution from elevated tank is controlled to 9m3Respectively entering a mixed liquid concentration tank and a parallel flow tank;
(6) and (4) allowing the flocculated mixed solution prepared in the step (5) to enter a primary clarifying barrel 8 for clarification and sedimentation treatment, controlling the retention time of the mixed solution in the primary clarifying barrel 8 for 11 hours to finally obtain supernatant with turbidity of 100ppm, conveying the supernatant to a calcium removal tower through a primary brine pump 9 to remove calcium, and removing primary mud from a mud washing barrel to wash mud.
Table 3: example 3 compares the data with the conventional crude brine magnesium removal plant operation.
Figure 535085DEST_PATH_IMAGE004
Example 4
Referring to fig. 1, the magnesium removal device for crude brine comprises a chemical precipitation aid device, a salt dissolving barrel 1, a crude brine launder 2, a front labyrinth groove 3, a mixed liquid centralized groove 4, a rear labyrinth groove 5, a first parallel launder 6, a second parallel launder 7, a primary clarifying barrel 8 and a primary brine pump 9 which are connected in sequence through pipelines; the front curve groove is provided with a lime milk pipeline interface 3-1. The chemical precipitation aid device comprises a precipitation aid tank 10, a precipitation aid pump 11 and a precipitation aid elevated tank 12 which are sequentially connected, wherein the precipitation aid tank is provided with a polyacrylamide feeding port 10-1 and a refined salt water feeding port 10-2, a liquid outlet pipeline of the precipitation aid elevated tank 12 is divided into two paths, one path is connected to the mixed liquid concentration tank 4, and the other path is divided into two paths which are respectively connected to a first precipitation aid solution feeding port 6-1 and a second precipitation aid solution feeding port 7-1 of the parallel flow tank; the outlet pipeline of the settling agent elevated tank is provided with a flowmeter 14, and the settling agent elevated tank is also provided with an overflow return pipeline 13 connected to the settling agent tank 10.

Claims (5)

1. The method for removing magnesium from crude brine comprises a salt melting barrel, a crude brine launder, a front labyrinth groove, a mixed solution concentration groove, a rear labyrinth groove, a parallel launder and a primary clarifying barrel which are sequentially connected through pipelines, and is characterized by comprising the following steps of:
(1) feeding the refined brine and the polyacrylamide into a settling agent tank, and stirring to fully dissolve the polyacrylamide to obtain a settling agent solution with the mass concentration of 0.8-1.0 per mill;
(2) pumping the settling agent solution obtained in the step (1) to a settling agent elevated tank through a settling agent pump, wherein the settling agent elevated tank adopts high liquid level reflux operation, so that part of the settling agent solution flows back to a settling agent tank through an overflow pipeline, and the reflux ratio is controlled to be 30-40%;
(3) meanwhile, raw salt and mixed water enter a salt dissolving barrel to be dissolved to prepare crude salt water, wherein the salt content of the crude salt water is controlled to be 108-108.5 ti;
(4) step by stepThe crude salt water prepared in the step (3) enters a front curve groove through a crude salt water groove, lime milk with the concentration of 150-160 ti is added to be fully mixed with the crude salt water for magnesium removal reaction, and the flow of the lime milk is controlled to be 15-20m3The residence time of the crude brine in the labyrinth groove is controlled to be 30-50s, and the surplus ash in the mixed liquid of the crude brine and the lime milk is controlled to be 0.1-0.15 ti;
(5) allowing the mixed solution prepared in the step (4) to enter a mixed solution collecting tank, adding 0.8-1.0 per mill of settling agent solution obtained in the step (2), allowing the mixed solution to flow through a rear labyrinth tank for continuous flocculation, adding settling agent solution for further flocculation when the mixed solution flows through parallel flow tanks, and flocculating fine magnesium hydroxide suspended matters into large flocs; the flow of the settling agent solution from the elevated tank is controlled to be 8-9m3Respectively entering a mixed liquid concentration tank and a parallel flow tank;
(6) and (4) allowing the flocculated mixed solution prepared in the step (5) to enter a primary clarifying barrel for clarifying and settling treatment, controlling the retention time of the mixed solution in the primary clarifying barrel for 10-12 hours, and finally obtaining supernatant with turbidity of 80-100 ppm, removing calcium from the supernatant by a calcium removal tower through a primary brine pump, and removing mud from a mud washing barrel.
2. The process for removing magnesium from crude brine according to claim 1, wherein in the step (1), the temperature of refined brine for dissolving and precipitating agent is controlled to be 40-45 ℃.
3. The magnesium removal device for crude brine for realizing the method of claim 1 or 2 is characterized by comprising a chemical precipitation aid device, a salt dissolving barrel, a crude brine launder, a front curve groove, a mixed solution collecting groove, a rear curve groove, a parallel launder and a primary clarifying barrel which are sequentially connected through pipelines; the front curve groove is provided with a lime milk pipeline interface; the settling agent dissolving device comprises a settling agent tank, a settling agent pump and a settling agent head tank which are sequentially connected, wherein the settling agent tank is provided with a stirring function and is provided with a settling agent feeding port and a refined brine feeding port, a liquid outlet pipeline of the settling agent head tank is divided into two paths, one path is connected to the mixed liquid concentration tank, and the other path is divided into two paths which are respectively connected to the settling agent solution feeding ports of the parallel flow tanks.
4. The magnesium removal device for crude brine according to claim 3, wherein a flowmeter is arranged on a liquid outlet pipeline of the settling agent elevated tank.
5. The magnesium removal device for crude brine according to claim 3, wherein the settling agent head tank is provided with an overflow return line connected to the settling agent tank.
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GB1519571A (en) * 1976-01-30 1978-08-02 Allied Chem Brine purification process
CN1021963C (en) * 1989-12-30 1993-09-01 中南工业大学 Method for removing magnesium from sodium chloride solution
DE10334521A1 (en) * 2003-07-29 2005-02-24 P & W Invest Vermögensverwaltungsgesellschaft mbH Flocculant, process for its preparation and its use
CN1254437C (en) * 2004-09-17 2006-05-03 覃德光 Method of refining salt solution
CN110697935A (en) * 2019-10-17 2020-01-17 青海盐湖工业股份有限公司 Refining system and refining method for byproduct brine
CN112374509B (en) * 2020-11-19 2023-05-09 山东海天生物化工有限公司 Refining process of refined brine for sodium carbonate production

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