CN110963521A - Extraction process of calcium chloride in yellow brine salt-making mother liquor - Google Patents
Extraction process of calcium chloride in yellow brine salt-making mother liquor Download PDFInfo
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- CN110963521A CN110963521A CN201911390050.4A CN201911390050A CN110963521A CN 110963521 A CN110963521 A CN 110963521A CN 201911390050 A CN201911390050 A CN 201911390050A CN 110963521 A CN110963521 A CN 110963521A
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Abstract
The invention belongs to the technical field of resource utilization of yellow brine mother liquor, and particularly relates to a process for extracting calcium chloride from yellow brine mother liquor. The process comprises the steps of 1) extracting bromine from yellow brine mother liquor, and pumping the yellow brine mother liquor into a magnesium removal reaction barrel by a pump to remove magnesium; 2) the pretreated liner water, namely the clear liquid in the step 1), reversely flows into a triple-effect evaporation system, namely sequentially passes through a III-effect evaporator, a II-effect evaporator and an I-effect evaporator; the feed liquid of the I-effect evaporator is evaporated and concentrated to CaCl2.2H2Cooling and tabletting after the mass concentration of O is 60-72%; 3) the concentrated solution after I-effect evaporation and deep concentration enters a flaking machine to obtain solid flaky CaCl2.2H2And O. The invention has reasonable process, stable operation, difficult scaling and greatly reduced operation cost, can realize the comprehensive utilization of resources, changes waste into valuable and has good economic benefit and environmental benefit.
Description
Technical Field
The invention belongs to the technical field of resource utilization of yellow brine mother liquor, and particularly relates to a process for extracting calcium chloride from yellow brine mother liquor.
Background
Common salt is an indispensable substance in human life, and is classified into sea salt, well salt, mineral salt, lake salt, earth salt and the like according to different sources. The main components of the salt are sodium chloride, and the sodium chloride content of well salt and mineral salt specified by the state is not less than 95%.
The natural brine is one of the main raw materials for well salt production in the thousand years of salt industry history in China. In China, natural brine salt chemical production enterprises represented by black brine of tribute Sichuan, Neijiang, and yellow brine of Penglai Sichuan and Leshan are formed. Compared with artificial bittern, the yellow bittern has relatively low sodium chloride content and is rich in Ca, Mg, Ba, Sr, K, Br, I and other chemical elements. Along with the evaporation of salt production, chemical elements are continuously enriched and can influence the energy consumption, the operation rate and the like of a salt production device, so that the salt production mother liquor is concentrated to a certain concentration and must be discharged out of the device, and the direct discharge can cause resource waste and environmental pollution.
In recent years, with the increasing national resource utilization and environmental protection policy, the effective treatment and comprehensive utilization of yellow brine mother liquor have become a particular concern for governments and yellow brine enterprises. In addition, the productivity of the salt manufacturing industry is greatly improved, the supply and demand relationship is shield, the single salt manufacturing enterprise has poor risk resistance, chemical elements such as calcium, barium, strontium, bromine, iodine and the like in the yellow bittern are important chemical raw materials, the product price is greatly improved, and the benefit is obvious. Therefore, the comprehensive utilization of the natural yellow brine salt-making mother liquor not only has environmental benefits, but also has certain economic benefits and social benefits.
Disclosure of Invention
The invention provides a process for extracting calcium chloride from yellow brine salt-making mother liquor according to the technical problems. The process mainly aims at the problem that a large amount of high-salt mother liquor generated in the production process of yellow brine is not stably treated, and the high-salt mother liquor mainly contains CaCl2Produced into CaCl2.2H2O is sold as a product.
CaCl2.2H2The O product is widely applied to the fields of chemical industry, shale gas exploitation and the like. Thus changing waste into valuable, not only having a ringEnvironmental benefit, and also has certain economic benefit and social benefit.
The specific technical scheme of the invention is as follows:
a process for extracting calcium chloride from yellow bittern salt-making mother liquor comprises three steps of gallbladder water pretreatment, triple-effect evaporation concentration desalination and cooling flaking.
The method comprises the following specific steps:
1) and pretreatment of the gallbladder water: and (3) extracting bromine from the yellow brine mother liquor, pumping into a magnesium removal reaction barrel by using a pump, synchronously adding lime powder and the bromine mother liquor into the magnesium removal reaction barrel by using a screw metering feeder, and adjusting the pH value of the solution to 9-10. Stirring for reaction, transferring to a magnesium-removing transfer barrel for further reaction and sedimentation to generate solid precipitate impurities of magnesium and other alkaline insoluble substances, pumping into a filter press for filter pressing after complete reaction, removing clear liquid from a clear liquid barrel for storage, mixing and stirring filter residues with white water, and pumping the mixture to a boiler desulfurization treatment section by a residue slurry pump.
The purpose of the pretreatment of the gall-bladder water is to remove magnesium and other alkaline insoluble substances which are easy to scale in the gall-bladder water, influence subsequent stable operation and influence product quality, namely 'magnesium removal'.
The main reaction is as follows:
CaO+H2O＝Ca(OH)2
Ca(OH)2+MgCl2＝Mg(OH)2↓+CaCl2
3Ca(OH)2+2FeCl3＝2Fe(OH)3↓+3CaCl2
Ca(OH)2+FeCl2＝Fe(OH)2↓+CaCl2
pumping solid precipitate impurities of magnesium hydroxide and other alkaline insoluble substances formed in the reaction barrel into a plate-and-frame filter press by a pump for filter pressing, removing clear liquid from a clear liquid barrel for storage, mixing and stirring filter residues by white water, and pumping the filter residues to a boiler desulfurization treatment section by a residue slurry pump. The magnesium ion content in the bile can be controlled below 10mg/L through the pretreatment step.
The preferred mechanism of lime as the magnesium removing agent is mainly as follows: the addition of lime can precipitate out magnesium ions and iron ions in the liner water, accelerate precipitation, improve the concentration of the liner water and adjust the pH value of the liner water entering the tank.
2) Triple-effect evaporation, concentration and desalination: the pretreated gall bladder water (23-28 wt% of calcium chloride) is preheated to 55-65 ℃ and then enters a multi-effect evaporation system in a countercurrent mode, namely sequentially passes through a III-effect evaporator, a II-effect evaporator, a horizontal screw centrifuge and an I-effect evaporator. The second effect evaporator and the third effect evaporator crystallize and desalt the solution, and the first effect evaporator makes the crystallized and desalted clear calcium chloride solution deeply concentrated. When the calcium chloride content in the solution is evaporated and concentrated to about 42-45 wt% by the effects II and III, the sodium chloride in the solution is completely crystallized and separated out, and the salt removed by a horizontal screw centrifuge is recycled to a salt production system. Naturally settling, centrifugally separating and desalting to obtain clear calcium chloride solution, and deeply concentrating in I-effect evaporator. And (3) deeply concentrating the first-effect evaporator to 60-72% of calcium chloride concentration, and then performing a cooling flaking process. The temperature of the I effect liquid is controlled to be 170-180 ℃, the temperature of the II effect liquid is controlled to be 105-115 ℃, and the temperature of the III effect liquid is controlled to be 65-75 ℃.
Preferably, the steam generated by the I-effect evaporator can be supplied to the II-effect evaporator, and the steam generated by the II-effect evaporator can be supplied to the III-effect evaporator, so that energy can be saved.
Preferably, the salt slurry generated by the II-effect evaporator returns to the III-effect evaporator, the salt generated by the III-effect evaporator after being separated by the centrifugal machine can return to the salt production system, and the mother liquor returns to the III-effect evaporator.
3) And (3) cooling and tabletting: the concentrated solution after I effect evaporator degree of depth is concentrated gets into the pelleter of cooling film-making system, and the principle is: circulating water or industrial water is fed into the tabletting machine, the concentrated solution of the effect I is cooled to about 30-50 ℃, and CaCl in liquid state is added2CaCl in solid flake form2.2H2And O, and then packaging for sale as a product.
The positive effects of the invention are as follows:
the invention adopts the technical scheme of gallbladder water pretreatment, triple-effect evaporation concentration desalination and cooling flaking. The lime powder is adopted to remove magnesium and other alkaline insoluble substances which are easy to scale in the gall water, influence subsequent stable operation and influence product quality, so that continuous, long-period and stable operation of subsequent processes is ensured, and meanwhile, the improvement is realizedThe purity of the calcium chloride dihydrate product and the produced CaCl2.2H2And the O is taken as a product to be sold, so that the economic benefit of the enterprise is increased.
The evaporation and concentration of the process adopts a scheme of triple-effect evaporation, concentration and desalination, fully utilizes the characteristics of different solubilities of sodium chloride and calcium chloride and different solubilities along with temperature change for desalination, comprehensively exerts the wide adaptability of multiple effects in various concentrations, particularly in high concentration and high boiling point rise, has more reasonable process and greatly reduces the operation cost.
And thirdly, the process has reasonable design, stable operation, difficult scaling and greatly reduced operation cost, can realize the comprehensive utilization of resources, changes waste into valuable and has good economic benefit and environmental benefit.
Description of the drawings:
FIG. 1 is a schematic flow chart of the process for extracting calcium chloride from the yellow brine salt-making mother liquor.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments for the purpose of making the objects, technical solutions and advantages of the present invention more apparent, but it should not be construed that the scope of the above-described subject matter of the present invention is limited to the following examples.
In the following examples,%, unless otherwise specified, all represent wt%.
Example 1:
a large amount of mother liquor is generated in the production process of yellow bittern salt of Sichuan xx salinization Co., Ltd, and a large amount of calcium chloride concentrated solution (bromine extraction mother liquor for short) is generated after bromine extraction of the mother liquor. The mother liquor for extracting bromine mainly contains CaCl2305g/L(23％)、NaCl55.63g/L、MgCl229.65g/L、FeCl313.23mg/L、FeCl28.55 mg/L. Pumping the bromine extraction mother liquor into a magnesium removal reaction barrel by a pump, synchronously adding lime powder and the bromine mother liquor into the magnesium removal reaction barrel from a storage bin through a screw metering feeder, and adjusting the pH value of the solution to 9.0. The main reaction is as follows:
CaO+H2O＝Ca(OH)2
Ca(OH)2+MgCl2＝Mg(OH)2↓+CaCl2
3Ca(OH)2+2FeCl3＝2Fe(OH)3↓+3CaCl2
Ca(OH)2+FeCl2＝Fe(OH)2↓+CaCl2
pumping magnesium hydroxide and other insoluble solid precipitate impurities formed in the reaction barrel into a plate-and-frame filter press by a pump for filter pressing, removing clear liquid from a clear liquid barrel for storage, mixing and stirring filter residues by white water (clear water), and pumping the filter residues to a boiler desulfurization treatment section by a slag slurry pump. The concentration of calcium chloride in the gall-bladder water is controlled to be increased to 337.83g/L (26 percent) by the process, and FeCl is added3And FeCl2The magnesium ion content was not detected, but was controlled to 10mg/L or less.
Preheating pretreated gall bladder water (26 wt% of calcium chloride) to 58 ℃, then feeding the gall bladder water into a III-effect evaporator of a multi-effect evaporation system in a countercurrent mode, concentrating the calcium chloride concentration of the gall bladder water to 32 wt%, then transferring the gall bladder water into a II-effect evaporator, discharging a concentrated solution into a centrifugal separation system for desalination when the II-effect evaporation is concentrated to 42 wt% (at the moment, all calcium chloride in the solution is crystallized and separated out), preheating the desalted clear calcium chloride solution to 165 ℃, then feeding the clear calcium chloride solution into the I-effect evaporator for deep concentration, and discharging the clear calcium chloride solution into a flaker for flaking when the calcium chloride is concentrated to 68 wt%. The temperature of the I effect liquid is controlled to be 180 ℃, the temperature of the II effect liquid is controlled to be 106 ℃, and the temperature of the III effect liquid is controlled to be 69 ℃.
Circulating water or industrial water is fed into the flaker, the concentrated solution of the effect I is cooled to about 40 ℃, and CaCl in liquid state is added2CaCl in solid flake form2.2H2And O, and then packaging for sale as a product.
By the process, the concentration of calcium chloride in the bile water after bromine extraction of the salt production mother liquor is increased from 23% to 26%, the yield can be increased, and the consumption can be reduced. The pH value of the water entering the tank liner is 9.0, so that the corrosion probability of equipment can be effectively reduced; magnesium ions in the bladder water can be controlled below 10ppm, iron ions can be detected, the phenomena of pipe blockage due to scaling and unqualified product quality caused by magnesium ions and the like are avoided, the heat transfer efficiency is improved, and the cleaning period is over 3 months; produced CaCl2.2H2And O meets the industrial calcium chloride standard, and is taken as a product for sale, so that the waste is changed into valuable, and the economic benefit of an enterprise is increased.
Example 2:
a large amount of mother liquor is generated in the production process of yellow bittern salt of Sichuan xx salinization Co., Ltd, and a large amount of calcium chloride concentrated solution (bromine extraction mother liquor for short) is generated after bromine extraction of the mother liquor. The mother liquor for extracting bromine mainly contains CaCl2305g/L(23％)、NaCl55.63g/L、MgCl229.65g/L、FeCl313.23mg/L、FeCl28.55 mg/L. Pumping the bromine extraction mother liquor into a magnesium removal reaction barrel by a pump, synchronously adding lime powder and the bromine mother liquor into the magnesium removal reaction barrel from a storage bin through a screw metering feeder, and adjusting the pH value of the solution to 9.5. The main reaction is as follows:
CaO+H2O＝Ca(OH)2
Ca(OH)2+MgCl2＝Mg(OH)2↓+CaCl2
3Ca(OH)2+2FeCl3＝2Fe(OH)3↓+3CaCl2
Ca(OH)2+FeCl2＝Fe(OH)2↓+CaCl2
pumping magnesium hydroxide and other insoluble solid precipitate impurities formed in the reaction barrel into a plate-and-frame filter press by a pump for filter pressing, removing clear liquid from a clear liquid barrel for storage, mixing and stirring filter residues by white water, and pumping the filter residues to a boiler desulfurization treatment section by a residue slurry pump. The concentration of calcium chloride in the gall-bladder water is controlled to be increased to 345.05g/L (26.5 percent) by the process, and FeCl is added3And FeCl2The magnesium ion content was not detected, and was controlled to 5mg/L or less.
Preheating pretreated gall bladder water (26.5 wt percent of calcium chloride) to 62 ℃, then feeding the gall bladder water into a III-effect evaporator of a multi-effect evaporation system in a countercurrent mode, concentrating the calcium chloride concentration of the gall bladder water to 32 percent, transferring the gall bladder water into a II-effect evaporator, discharging concentrated solution into a centrifugal separation system for desalination when the II-effect evaporation is concentrated to 42 percent (at the moment, calcium chloride in the solution is completely crystallized and separated out), preheating the desalted calcium chloride clear solution to 170 ℃, then feeding the calcium chloride clear solution into the I-effect evaporator for deep concentration, and discharging the calcium chloride into a flaker for flaking when the calcium chloride is concentrated to 68 percent. The temperature of the I effect liquid is 180 ℃, the temperature of the II effect liquid is 106 ℃, and the temperature of the III effect liquid is 69 ℃.
Circulating water or industrial water is fed into the flaker, the concentrated solution of the effect I is cooled to about 30-50 ℃, and CaCl in liquid state is added2In the form of solid flakesaCl2.2H2And O, and then packaging for sale as a product.
By the process, the concentration of calcium chloride in the bile water after bromine extraction of the salt production mother liquor is increased from 23% to 26.5%, the yield can be increased, and the consumption can be reduced. The pH value of the water entering the tank liner is 9.5, so that the corrosion probability of equipment can be effectively reduced; the magnesium ions in the water can be controlled below 5ppm, the iron ions can be detected, the phenomena of pipe blockage due to scaling and unqualified product quality caused by magnesium ions and the like are avoided, the heat transfer efficiency is improved, and the cleaning period is over 5 months. Produced CaCl2.2H2And O meets the standard of industrial calcium chloride products, and is taken out as a product, so that the waste is changed into valuable, and the economic benefit of an enterprise is increased.
Comparative example 1:
a large amount of mother liquor is generated in the production process of yellow bittern salt of Sichuan xx salinization Co., Ltd, and a large amount of calcium chloride concentrated solution (bromine extraction mother liquor for short) is generated after bromine extraction of the mother liquor. The mother liquor for extracting bromine mainly contains CaCl2305g/L(23％)、NaCl55.63g/L、MgCl229.65g/L、FeCl313.23mg/L、FeCl28.55 mg/L. Pumping the bromine extraction mother liquor into a magnesium removal reaction barrel by a pump, synchronously adding lime powder and the bromine mother liquor into the magnesium removal reaction barrel from a storage bin through a screw metering feeder, and adjusting the pH value of the solution to 8.0. The main reaction is as follows:
CaO+H2O＝Ca(OH)2
Ca(OH)2+MgCl2＝Mg(OH)2↓+CaCl2
3Ca(OH)2+2FeCl3＝2Fe(OH)3↓+3CaCl2
Ca(OH)2+FeCl2＝Fe(OH)2↓+CaCl2
pumping magnesium hydroxide and other insoluble solid precipitate impurities formed in the reaction barrel into a plate-and-frame filter press by a pump for filter pressing, removing clear liquid from a clear liquid barrel for storage, mixing and stirring filter residues by white water, and pumping the filter residues to a boiler desulfurization treatment section by a residue slurry pump. The content of magnesium ions in the bile water is reduced and kept above 100ppm by the process, and the magnesium removal effect is not ideal.
Preheating pretreated gall bladder water (24.5 percent of calcium chloride) to 62 ℃, then feeding the gall bladder water into a III-effect evaporator of a multi-effect evaporation system in a countercurrent mode, concentrating the calcium chloride concentration of the gall bladder water to 32 percent, transferring the gall bladder water into a II-effect evaporator, discharging concentrated solution into a centrifugal separation system for desalination when the II-effect evaporation is concentrated to 42 percent (at the moment, calcium chloride in the solution is completely crystallized and separated out), preheating the desalted calcium chloride clear solution to 170 ℃, then feeding the calcium chloride clear solution into the I-effect evaporator for deep concentration, and discharging the calcium chloride into a flaker for flaking when the calcium chloride is concentrated to 68 percent. The temperature of the I effect liquid is 180 ℃, the temperature of the II effect liquid is 106 ℃, and the temperature of the III effect liquid is 69 ℃.
Circulating water or industrial water is fed into the flaker, the concentrated solution of the effect I is cooled to about 30-50 ℃, and CaCl in liquid state is added2CaCl in solid flake form2.2H2And O, and then packaging for sale as a product.
By the process, the magnesium ions in the bile water after the bromine extraction of the salt production mother liquor are over 100ppm, although CaCl can also be produced2.2H2O product, but the appearance and purity of the product are obviously reduced, the energy consumption is increased, the cleaning period of the equipment is obviously shortened, and the production system is unstable.
Comparative example 2:
a large amount of mother liquor is generated in the production process of yellow bittern salt of Sichuan xx salinization Co., Ltd, and a large amount of calcium chloride concentrated solution (bromine extraction mother liquor for short) is generated after bromine extraction of the mother liquor. The mother liquor for extracting bromine mainly contains CaCl2305g/L(23％)、NaCl55.63g/L、MgCl229.65g/L、FeCl313.23mg/L、FeCl28.55 mg/L. Directly enters a triple-effect evaporation system without pretreatment.
By the process, the temperature of the effect liquid I is not 170-180 ℃; although CaCl can also be produced2.2H2O, but does not meet the standard of industrial calcium chloride products, and increases the subsequent treatment cost; the pH value in the tank is less than 5, and the corrosion probability of equipment is high; the production is unstable, the labor intensity is high, and the energy consumption is high.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. A process for extracting calcium chloride from yellow brine salt-making mother liquor is characterized by comprising three steps of gallbladder water pretreatment, triple-effect evaporation concentration desalination and cooling flaking, and comprises the following specific steps:
1) and pretreatment of the gallbladder water: extracting bromine from the yellow brine mother liquor, pumping the yellow brine mother liquor into a magnesium removal reaction barrel by using a pump, synchronously adding lime powder into the magnesium removal reaction barrel together with the bromine mother liquor by using a screw metering feeder, stirring for reaction, transferring the mixture into a magnesium removal transfer barrel for further reaction and sedimentation to generate solid precipitate impurities of magnesium and other alkaline insoluble substances, pumping the mixture into a filter press for filter pressing after the reaction is completed, removing a clear solution from the clear solution for storage, mixing and stirring filter residues by using white water, and pumping the filter residues to a boiler desulfurization treatment section by using a residue slurry pump;
2) triple-effect evaporation, concentration and desalination: the pretreated liner water, namely the clear liquid in the step 1), reversely flows into a triple-effect evaporation system, namely sequentially passes through a III-effect evaporator, a II-effect evaporator and an I-effect evaporator; the feed liquid of the I-effect evaporator is evaporated and concentrated to CaCl2.2H2Cooling and tabletting after the mass concentration of O is 60-72%;
3) and (3) cooling and tabletting: the concentrated solution after I-effect evaporation and deep concentration enters a flaking machine of a cooling flaking system, circulating water or industrial water is introduced into the flaking machine, the concentrated solution is cooled to 30-50 ℃, and liquid CaCl is obtained2CaCl in solid flake form2.2H2And O, and then packaging for sale as a product.
2. The process for extracting calcium chloride from the yellow brine salt mother liquor as claimed in claim 1, wherein: the mass percentage of the calcium chloride in the pretreated gall bladder water is 23-28%.
3. The process for extracting calcium chloride from the yellow brine salt mother liquor as claimed in claim 1, wherein: and (3) adding the lime powder and the bromine mother liquor into a magnesium removal reaction barrel synchronously through a screw metering feeder, and adjusting the pH value of the solution to 9-10.
4. The process for extracting calcium chloride from the yellow brine salt mother liquor as claimed in claim 1, wherein: the pretreatment step controls the content of magnesium ions in the bile to be below 10 mg/L.
5. The process for extracting calcium chloride from the yellow brine salt mother liquor as claimed in claim 1, wherein: preheating to 55-65 ℃, and then feeding the mixture into a multi-effect evaporation system in a countercurrent manner.
6. The process for extracting calcium chloride from the yellow brine salt mother liquor as claimed in claim 1, wherein: a horizontal centrifuge is arranged between the second-effect evaporator and the first-effect evaporator, and the liquid after centrifugal separation enters the first-effect evaporator.
7. The process for extracting calcium chloride from the yellow brine salt mother liquor as claimed in claim 1, wherein: in the first-effect evaporator, the calcium chloride solution is deeply concentrated, and evaporation, crystallization and desalination are carried out in the second-effect evaporator and the third-effect evaporator, wherein the temperature of the first-effect liquid is controlled to be 170-180 ℃, the temperature of the second-effect liquid is controlled to be 105-115 ℃, and the temperature of the third-effect liquid is controlled to be 65-75 ℃.
8. The process for extracting calcium chloride from the yellow brine salt mother liquor as claimed in claim 1, wherein: and after the solution passes through a second-effect evaporator and a third-effect evaporator, evaporating and concentrating the solution until the mass concentration of calcium chloride is 42-45%.
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