CN113979451A - Preparation method of ecological well mineral salt - Google Patents

Preparation method of ecological well mineral salt Download PDF

Info

Publication number
CN113979451A
CN113979451A CN202111306886.9A CN202111306886A CN113979451A CN 113979451 A CN113979451 A CN 113979451A CN 202111306886 A CN202111306886 A CN 202111306886A CN 113979451 A CN113979451 A CN 113979451A
Authority
CN
China
Prior art keywords
steam
reaction kettle
supplied
salt
carbon dioxide
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202111306886.9A
Other languages
Chinese (zh)
Inventor
裴庆军
张英仓
曹伟
王淑刚
党召芳
李梦夏
赵振
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shandong Daiyue Salt Co ltd
Original Assignee
Shandong Daiyue Salt Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shandong Daiyue Salt Co ltd filed Critical Shandong Daiyue Salt Co ltd
Priority to CN202111306886.9A priority Critical patent/CN113979451A/en
Publication of CN113979451A publication Critical patent/CN113979451A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • C01D3/04Chlorides
    • C01D3/08Preparation by working up natural or industrial salt mixtures or siliceous minerals
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L27/00Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/40Table salts; Dietetic salt substitutes
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/60Optical properties, e.g. expressed in CIELAB-values
    • C01P2006/65Chroma (C*)
    • 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

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Geology (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Inorganic Chemistry (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Seasonings (AREA)

Abstract

The invention discloses a preparation method of ecological well mineral salt, which takes natural rock salt collected from the underground with the depth of 1000 meters as a raw material, carries out three-step heating under the condition of introducing carbon dioxide, combines a five-effect evaporator for evaporation and crystallization, collects salt slurry, centrifugally dehydrates and dries to obtain the ecological well mineral salt. In the preparation process, the invention avoids the use of sodium hydroxide, sodium carbonate and other chemicals, and has the advantages of purity, no addition and high product quality.

Description

Preparation method of ecological well mineral salt
Technical Field
The invention relates to a preparation method of ecological well mineral salt. Belongs to the technical field of edible salt processing.
Background
The well mineral salt is salt produced by pumping underground natural brine through well drilling and salt produced by processing mined underground rock salt, and the production process comprises two major parts of mining and salt production. Decocting with round or flat pot for long time. Since the end of the 19 th century, advanced technologies such as vacuum evaporation, hot-pressing evaporation, combination of vacuum and hot pressing and the like are gradually adopted for salt preparation. For mining, underground natural brine is pumped by a bailing method, a gas lift method or a submerged brine pump; rock salt is mined by well roadways (dry mining) and water-soluble mining according to the geology of an ore deposit, occurrence conditions and the grade. The rock salt is formed by precipitation and layering in the crust through complex geological movement after ancient seawater or lake water is dried, has high purity and less impurities, and is very popular with consumers.
However, in the prior art, in the process of refining salt products by using rock salt as a raw material, sodium hydroxide, sodium carbonate and the like are required to be added into raw material brine for removing calcium and magnesium ions in the brine, and simultaneously, precipitation-assisting agents, namely polyacrylamide and sodium polyacrylate, are added for accelerating precipitation, so that various chemicals which are not beneficial to human bodies and are even harmful are added in the production process. The production of refined salt usually requires purification, evaporation, crystallization, drying, packaging and other processes, and the operation process is complicated, the production cost is relatively high, and the product purity is limited to a certain extent. Therefore, the quality of the edible salt is ensured on the premise of reducing the use of chemicals, natural trace elements rich in nature are reserved, and the concept of 'ecological salt' which is highly advocated by the current market is gradually formed.
Patent CN104973611B discloses a method for preparing salting salt, which comprises using saturated brine as raw material, purifying with purifying agent, evaporating, concentrating and crystallizing with evaporator to obtain high-purity salting salt with large particles, wherein brine purification is realized by adding chemicals such as sodium hydroxide, sodium carbonate and calcium chloride, which obviously does not conform to the concept of "ecological salt".
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of the ecological well mineral salt, which avoids the use of chemicals and has high product quality.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of ecological well mineral salt comprises the following specific steps:
(1) adding natural rock salt into a reaction kettle, heating to 650-750 ℃, introducing carbon dioxide into the reaction kettle in a heat preservation state, and discharging substances in a molten state in the reaction kettle through a discharge port;
(2) heating to 799 ℃, introducing carbon dioxide into the reaction kettle in a heat preservation state, and discharging substances in a molten state in the reaction kettle through a discharge hole;
(3) heating to 820-830 ℃, introducing carbon dioxide into the reaction kettle in a heat preservation state, collecting substances in a molten state from a discharge hole of the reaction kettle, cooling to obtain a solid, adding the solid into water, and stirring to dissolve to obtain brine;
(4) and finally pumping the brine into a five-effect evaporator for evaporation and crystallization, wherein the five-effect discharge amount is 15%, 30%, 45%, 60% and 50% of the corresponding feed amount in sequence, collecting salt slurry, centrifugally dewatering and drying to obtain the ecological well mineral salt.
Preferably, in step (1), the natural rock salt is collected from the underground at a depth of 1000 m.
Preferably, in the step (1), the heating rate is 8-10 ℃/min, the heat preservation time is 35-45 min, and the flow rate of carbon dioxide is 5-8 m/s.
Preferably, in the step (2), the temperature rising rate is 4-6 ℃/min, the heat preservation time is 30-40 min, and the flow rate of carbon dioxide is 10-12 m/s.
Preferably, in the step (3), the heating rate is 0.5-0.8 ℃/min, the heat preservation time is 50-60 min, and the flow rate of the carbon dioxide is 3-5 m/s.
Preferably, in the step (3), the cooling method specifically comprises the following steps: and (3) cooling the obtained molten substance by air circulation, and collecting the obtained solid from the space between double-layer screens by passing through double-layer screens of 10 meshes and 15 meshes in the cooling process.
Further preferably, the air circulation flow rate is 10-12 m/s.
Preferably, in the step (3), the weight ratio of the solid to the water is 1: 12 to 15.
Preferably, in the step (4), the process conditions of the five-effect evaporator are as follows: the steam pressure is 0.6-0.8 MPa, the air pressure is 0.2-0.3 MPa, the gas phase temperature is 100-110 ℃, and the liquid phase temperature is 105-115 ℃.
Further preferably, the steam supply mode of the five-effect evaporator is as follows: the production is stopped for less than 5 hours, and steam can be supplied once; the steam supply for 5-24 hours of production stop comprises two steps: 1/2 is supplied for the first time, and all the 1/2 can be supplied after 1 hour; stopping production for 24 hours to 72 hours, and supplying steam in three steps: 1/3 is supplied for the first time, 1/3 is supplied after 1 hour, and the supply is completed after another 1 hour; stopping production for more than 72 hours, and supplying steam in four steps: preheating the heating chamber with a small amount of steam for the first time, wherein the amount of the steam is 1/3 after 1 hour, 1/3 of the steam is supplied after another 1 hour, and the steam is completely supplied after another 1 hour, based on the condition that the pressure of the heating chamber is not raised.
Preferably, before the crystallization (salting out) of the effect liquid, the pollution is discharged from the salt foot once respectively to remove impurities precipitated from each effect.
The invention has the beneficial effects that:
the method comprises the steps of taking natural rock salt collected from the underground and with the depth of 1000 m as a raw material, carrying out three-step heating under the condition of introducing carbon dioxide, combining with a five-effect evaporator for evaporation and crystallization, collecting salt slurry, centrifugally dewatering and drying to obtain the ecological well mineral salt. In the preparation process, the use of sodium hydroxide, sodium carbonate and other chemicals is avoided, the product is pure and free of additives, and the product quality is high.
Specifically, the method comprises the steps of adding natural rock salt into a reaction kettle, heating to 650-750 ℃, introducing carbon dioxide into the reaction kettle in a heat preservation state, and discharging substances in a molten state in the reaction kettle through a discharge hole; heating to 799 ℃, introducing carbon dioxide into the reaction kettle in a heat preservation state, and discharging substances in a molten state in the reaction kettle through a discharge hole; heating to 820-830 ℃, introducing carbon dioxide into the reaction kettle in a heat preservation state, collecting substances in a molten state from a discharge hole of the reaction kettle, cooling to obtain a solid, adding the solid into water, and stirring to dissolve to obtain brine; and finally pumping the brine into a five-effect evaporator for evaporation and crystallization, wherein the five-effect discharge amount is 15%, 30%, 45%, 60% and 50% of the corresponding feed amount in sequence, collecting salt slurry, centrifugally dewatering and drying to obtain the ecological well mineral salt.
The invention adopts a three-step heating method, because the melting point of the sodium chloride is 801 ℃, the invention is controlled below 801 ℃ firstly, impurities lower than the melting point of the sodium chloride are removed, and carbon dioxide is introduced in the heat preservation process, which is beneficial to taking the impurities out of the reaction kettle. Heating step by step, namely heating to 650-750 ℃ firstly, then heating to 799 ℃ to be beneficial to fully removing impurities, then heating to 820-830 ℃ to fully melt and separate out sodium chloride, and keeping the temperature in the presence of carbon dioxide to be beneficial to removing high-melting-point impurities. The temperature rise rate is from fast to slow, which is beneficial to removing impurities in each step, thereby improving the product quality.
According to the invention, the brine is evaporated and crystallized through the five-effect evaporator, the five-effect discharge amount is controlled, the attachment of small molecular organic matters on the surface of sodium chloride is effectively avoided, and the product quality is further improved.
Detailed Description
The present invention will be further illustrated by the following examples, which are intended to be merely illustrative and not limitative.
Example 1:
a preparation method of ecological well mineral salt comprises the following specific steps:
(1) adding natural rock salt collected from the underground with the depth of 1000 m into a reaction kettle, heating to 650 ℃, introducing carbon dioxide into the reaction kettle in a heat preservation state, and discharging substances in a molten state in the reaction kettle through a discharge hole;
(2) heating to 799 ℃, introducing carbon dioxide into the reaction kettle in a heat preservation state, and discharging substances in a molten state in the reaction kettle through a discharge hole;
(3) heating to 830 ℃, introducing carbon dioxide into the reaction kettle in a heat preservation state, collecting substances in a molten state from a discharge hole of the reaction kettle, cooling to obtain a solid, adding 10kg of the solid into 120kg of water, and stirring to dissolve to obtain brine;
(4) and finally pumping the brine into a five-effect evaporator for evaporation and crystallization, wherein the five-effect discharge amount is 15%, 30%, 45%, 60% and 50% of the corresponding feed amount in sequence, collecting salt slurry, centrifugally dewatering and drying to obtain the ecological well mineral salt.
In the step (1), the heating rate is 10 ℃/min, the heat preservation time is 35 min, and the flow rate of carbon dioxide is 8 m/s.
In the step (2), the heating rate is 4 ℃/min, the heat preservation time is 40 min, and the flow rate of carbon dioxide is 10 m/s.
In the step (3), the heating rate is 0.8 ℃/min, the heat preservation time is 50 min, and the flow rate of carbon dioxide is 5 m/s.
In the step (3), the cooling method specifically comprises the following steps: the obtained molten material was cooled by air circulation (air circulation flow rate of 10m/s), and passed through a double-layer screen of 10 mesh and 15 mesh during cooling, and the obtained solid was collected from between the double-layer screen.
In the step (4), the process conditions of the five-effect evaporator are as follows: the vapor pressure is 0.8MPa, the air pressure is 0.2MPa, the gas phase temperature is 100 ℃, and the liquid phase temperature is 105 ℃.
The steam supply mode of the five-effect evaporator is as follows: the production is stopped for less than 5 hours, and steam can be supplied once; the steam supply for 5-24 hours of production stop comprises two steps: 1/2 is supplied for the first time, and all the 1/2 can be supplied after 1 hour; stopping production for 24 hours to 72 hours, and supplying steam in three steps: 1/3 is supplied for the first time, 1/3 is supplied after 1 hour, and the supply is completed after another 1 hour; stopping production for more than 72 hours, and supplying steam in four steps: preheating the heating chamber with a small amount of steam for the first time, wherein the amount of the steam is 1/3 after 1 hour, 1/3 of the steam is supplied after another 1 hour, and the steam is completely supplied after another 1 hour, based on the condition that the pressure of the heating chamber is not raised.
Before the crystallization (salting out) of the effect liquid, the pollution is discharged from the salt foot once respectively to remove the impurities precipitated from each effect.
Example 2:
a preparation method of ecological well mineral salt comprises the following specific steps:
(1) adding natural rock salt collected from the underground with the depth of 1000 m into a reaction kettle, heating to 750 ℃, introducing carbon dioxide into the reaction kettle in a heat preservation state, and discharging substances in a molten state in the reaction kettle through a discharge hole;
(2) heating to 799 ℃, introducing carbon dioxide into the reaction kettle in a heat preservation state, and discharging substances in a molten state in the reaction kettle through a discharge hole;
(3) heating to 820 ℃, introducing carbon dioxide into the reaction kettle in a heat preservation state, collecting substances in a molten state from a discharge port of the reaction kettle, cooling to obtain a solid, adding 10kg of the solid into 150kg of water, and stirring and dissolving to obtain brine;
(4) and finally pumping the brine into a five-effect evaporator for evaporation and crystallization, wherein the five-effect discharge amount is 15%, 30%, 45%, 60% and 50% of the corresponding feed amount in sequence, collecting salt slurry, centrifugally dewatering and drying to obtain the ecological well mineral salt.
In the step (1), the heating rate is 8 ℃/min, the heat preservation time is 45 min, and the flow rate of carbon dioxide is 5 m/s.
In the step (2), the heating rate is 6 ℃/min, the heat preservation time is 30 min, and the flow rate of carbon dioxide is 12 m/s.
In the step (3), the heating rate is 0.5 ℃/min, the heat preservation time is 60 min, and the flow rate of carbon dioxide is 3 m/s.
In the step (3), the cooling method specifically comprises the following steps: the obtained molten material was cooled by air circulation (air circulation flow rate of 12m/s), and passed through a double-layer screen of 10 mesh and 15 mesh during cooling, and the obtained solid was collected from between the double-layer screen.
In the step (4), the process conditions of the five-effect evaporator are as follows: the vapor pressure is 0.6MPa, the air pressure is 0.3MPa, the gas phase temperature is 110 ℃, and the liquid phase temperature is 115 ℃.
The steam supply mode of the five-effect evaporator is as follows: the production is stopped for less than 5 hours, and steam can be supplied once; the steam supply for 5-24 hours of production stop comprises two steps: 1/2 is supplied for the first time, and all the 1/2 can be supplied after 1 hour; stopping production for 24 hours to 72 hours, and supplying steam in three steps: 1/3 is supplied for the first time, 1/3 is supplied after 1 hour, and the supply is completed after another 1 hour; stopping production for more than 72 hours, and supplying steam in four steps: preheating the heating chamber with a small amount of steam for the first time, wherein the amount of the steam is 1/3 after 1 hour, 1/3 of the steam is supplied after another 1 hour, and the steam is completely supplied after another 1 hour, based on the condition that the pressure of the heating chamber is not raised.
Before the crystallization (salting out) of the effect liquid, the pollution is discharged from the salt foot once respectively to remove the impurities precipitated from each effect.
Example 3:
a preparation method of ecological well mineral salt comprises the following specific steps:
(1) adding natural rock salt collected from the underground with the depth of 1000 m into a reaction kettle, heating to 700 ℃, introducing carbon dioxide into the reaction kettle in a heat preservation state, and discharging substances in a molten state in the reaction kettle through a discharge hole;
(2) heating to 799 ℃, introducing carbon dioxide into the reaction kettle in a heat preservation state, and discharging substances in a molten state in the reaction kettle through a discharge hole;
(3) heating to 825 deg.C, introducing carbon dioxide into the reaction kettle under heat preservation, collecting molten substance from the discharge port of the reaction kettle, cooling to obtain solid, adding 10kg of the solid into 140kg of water, stirring and dissolving to obtain brine;
(4) and finally pumping the brine into a five-effect evaporator for evaporation and crystallization, wherein the five-effect discharge amount is 15%, 30%, 45%, 60% and 50% of the corresponding feed amount in sequence, collecting salt slurry, centrifugally dewatering and drying to obtain the ecological well mineral salt.
In the step (1), the heating rate is 9 ℃/min, the heat preservation time is 40 min, and the flow rate of carbon dioxide is 7 m/s.
In the step (2), the heating rate is 5 ℃/min, the heat preservation time is 35 min, and the flow rate of carbon dioxide is 11 m/s.
In the step (3), the heating rate is 0.7 ℃/min, the heat preservation time is 55 min, and the flow rate of carbon dioxide is 4 m/s.
In the step (3), the cooling method specifically comprises the following steps: the obtained molten material was cooled by air circulation (air circulation flow rate of 11m/s), and passed through a double-layer screen of 10 mesh and 15 mesh during cooling, and the obtained solid was collected from between the double-layer screen.
In the step (4), the process conditions of the five-effect evaporator are as follows: the vapor pressure is 0.7MPa, the air pressure is 0.25MPa, the gas phase temperature is 105 ℃, and the liquid phase temperature is 110 ℃.
The steam supply mode of the five-effect evaporator is as follows: the production is stopped for less than 5 hours, and steam can be supplied once; the steam supply for 5-24 hours of production stop comprises two steps: 1/2 is supplied for the first time, and all the 1/2 can be supplied after 1 hour; stopping production for 24 hours to 72 hours, and supplying steam in three steps: 1/3 is supplied for the first time, 1/3 is supplied after 1 hour, and the supply is completed after another 1 hour; stopping production for more than 72 hours, and supplying steam in four steps: preheating the heating chamber with a small amount of steam for the first time, wherein the amount of the steam is 1/3 after 1 hour, 1/3 of the steam is supplied after another 1 hour, and the steam is completely supplied after another 1 hour, based on the condition that the pressure of the heating chamber is not raised.
Before the crystallization (salting out) of the effect liquid, the pollution is discharged from the salt foot once respectively to remove the impurities precipitated from each effect.
Comparative example 1
A preparation method of ecological well mineral salt comprises the following specific steps:
(1) adding natural rock salt collected from the underground with the depth of 1000 m into a reaction kettle, heating to 830 ℃, introducing carbon dioxide into the reaction kettle in a heat preservation state, collecting substances in a molten state from a discharge port of the reaction kettle, cooling to obtain a solid, adding 10kg of the solid into 120kg of water, and stirring and dissolving to obtain brine;
(2) and finally pumping the brine into a five-effect evaporator for evaporation and crystallization, wherein the five-effect discharge amount is 15%, 30%, 45%, 60% and 50% of the corresponding feed amount in sequence, collecting salt slurry, centrifugally dewatering and drying to obtain the ecological well mineral salt.
In the step (1), the heating rate is 10 ℃/min, the heat preservation time is 50 min, and the flow rate of carbon dioxide is 8 m/s.
In the step (2), the process conditions of the five-effect evaporator are as follows: the vapor pressure is 0.8MPa, the air pressure is 0.2MPa, the gas phase temperature is 100 ℃, and the liquid phase temperature is 105 ℃.
The steam supply mode of the five-effect evaporator is as follows: the production is stopped for less than 5 hours, and steam can be supplied once; the steam supply for 5-24 hours of production stop comprises two steps: 1/2 is supplied for the first time, and all the 1/2 can be supplied after 1 hour; stopping production for 24 hours to 72 hours, and supplying steam in three steps: 1/3 is supplied for the first time, 1/3 is supplied after 1 hour, and the supply is completed after another 1 hour; stopping production for more than 72 hours, and supplying steam in four steps: preheating the heating chamber with a small amount of steam for the first time, wherein the amount of the steam is 1/3 after 1 hour, 1/3 of the steam is supplied after another 1 hour, and the steam is completely supplied after another 1 hour, based on the condition that the pressure of the heating chamber is not raised.
Before the crystallization (salting out) of the effect liquid, the pollution is discharged from the salt foot once respectively to remove the impurities precipitated from each effect.
Comparative example 2
A preparation method of ecological well mineral salt comprises the following specific steps:
(1) firstly, adding natural rock salt collected from the underground with the depth of 1000 m into a reaction kettle, heating to 650 ℃, preserving heat for 35 minutes, and discharging substances in a molten state in the reaction kettle through a discharge hole;
(2) heating to 799 ℃, preserving heat for 40 minutes, and discharging substances in a molten state in the reaction kettle through a discharge hole;
(3) heating to 830 ℃, preserving heat for 50 minutes, collecting substances in a molten state from a discharge hole of the reaction kettle, cooling to obtain a solid, adding 10kg of the solid into 120kg of water, and stirring to dissolve to obtain brine;
(4) and finally pumping the brine into a five-effect evaporator for evaporation and crystallization, wherein the five-effect discharge amount is 15%, 30%, 45%, 60% and 50% of the corresponding feed amount in sequence, collecting salt slurry, centrifugally dewatering and drying to obtain the ecological well mineral salt.
In the step (3), the cooling method specifically comprises the following steps: the obtained molten material was cooled by air circulation (air circulation flow rate of 10m/s), and passed through a double-layer screen of 10 mesh and 15 mesh during cooling, and the obtained solid was collected from between the double-layer screen.
In the step (4), the process conditions of the five-effect evaporator are as follows: the vapor pressure is 0.8MPa, the air pressure is 0.2MPa, the gas phase temperature is 100 ℃, and the liquid phase temperature is 105 ℃.
The steam supply mode of the five-effect evaporator is as follows: the production is stopped for less than 5 hours, and steam can be supplied once; the steam supply for 5-24 hours of production stop comprises two steps: 1/2 is supplied for the first time, and all the 1/2 can be supplied after 1 hour; stopping production for 24 hours to 72 hours, and supplying steam in three steps: 1/3 is supplied for the first time, 1/3 is supplied after 1 hour, and the supply is completed after another 1 hour; stopping production for more than 72 hours, and supplying steam in four steps: preheating the heating chamber with a small amount of steam for the first time, wherein the amount of the steam is 1/3 after 1 hour, 1/3 of the steam is supplied after another 1 hour, and the steam is completely supplied after another 1 hour, based on the condition that the pressure of the heating chamber is not raised.
Before the crystallization (salting out) of the effect liquid, the pollution is discharged from the salt foot once respectively to remove the impurities precipitated from each effect.
Test examples
With reference to GB/T5461-2016, the results of the related index investigation of the well mineral salts obtained in examples 1-3 and comparative examples 1-3 are shown in Table 1.
TABLE 1 investigation results of well mineral salt indexes
Figure BDA0003340638730000071
As can be seen from Table 1, the well mineral salt obtained in examples 1 to 3 has high whiteness, high sodium chloride content and low water insoluble content, and meets the national standards of edible salt.
Comparative example 1 replaces three-step heating with one-step heating, comparative example 2 does not introduce carbon dioxide, and the quality of the obtained well mineral salt is obviously poor, which shows that the step-by-step heating and the carbon dioxide have synergistic effect to improve the quality of the well mineral salt.
Although the present invention has been described with reference to the specific embodiments, it is not intended to limit the scope of the present invention, and various modifications and variations can be made by those skilled in the art without inventive changes based on the technical solution of the present invention.

Claims (10)

1. The preparation method of the ecological well mineral salt is characterized by comprising the following specific steps:
(1) adding natural rock salt into a reaction kettle, heating to 650-750 ℃, introducing carbon dioxide into the reaction kettle in a heat preservation state, and discharging substances in a molten state in the reaction kettle through a discharge port;
(2) heating to 799 ℃, introducing carbon dioxide into the reaction kettle in a heat preservation state, and discharging substances in a molten state in the reaction kettle through a discharge hole;
(3) heating to 820-830 ℃, introducing carbon dioxide into the reaction kettle in a heat preservation state, collecting substances in a molten state from a discharge hole of the reaction kettle, cooling to obtain a solid, adding the solid into water, and stirring to dissolve to obtain brine;
(4) and finally pumping the brine into a five-effect evaporator for evaporation and crystallization, wherein the five-effect discharge amount is 15%, 30%, 45%, 60% and 50% of the corresponding feed amount in sequence, collecting salt slurry, centrifugally dewatering and drying to obtain the ecological well mineral salt.
2. The method according to claim 1, wherein in step (1), the natural rock salt is collected from the underground at a depth of 1000 m.
3. The preparation method according to claim 1, wherein in the step (1), the temperature rise rate is 8-10 ℃/min, the heat preservation time is 35-45 min, and the flow rate of the carbon dioxide is 5-8 m/s.
4. The preparation method according to claim 1, wherein in the step (2), the temperature rise rate is 4-6 ℃/min, the heat preservation time is 30-40 min, and the flow rate of the carbon dioxide is 10-12 m/s.
5. The method according to claim 1, wherein in the step (3), the temperature rise rate is 0.5 to 0.8 ℃/min, the heat preservation time is 50 to 60 minutes, and the flow rate of the carbon dioxide is 3 to 5 m/s.
6. The preparation method according to claim 1, wherein in the step (3), the cooling is performed by: and (3) cooling the obtained molten substance by air circulation, and collecting the obtained solid from the space between double-layer screens by passing through double-layer screens of 10 meshes and 15 meshes in the cooling process.
7. The method according to claim 1, wherein in the step (3), the weight ratio of the solid to the water is 1: 12 to 15.
8. The preparation method according to claim 1, wherein in the step (4), the process conditions of the five-effect evaporator are as follows: the steam pressure is 0.6-0.8 MPa, the air pressure is 0.2-0.3 MPa, the gas phase temperature is 100-110 ℃, and the liquid phase temperature is 105-115 ℃.
9. The preparation method of claim 8, wherein the steam supply mode of the five-effect evaporator is as follows: the production is stopped for less than 5 hours, and steam can be supplied once; the steam supply for 5-24 hours of production stop comprises two steps: 1/2 is supplied for the first time, and all the 1/2 can be supplied after 1 hour; stopping production for 24 hours to 72 hours, and supplying steam in three steps: 1/3 is supplied for the first time, 1/3 is supplied after 1 hour, and the supply is completed after another 1 hour; stopping production for more than 72 hours, and supplying steam in four steps: preheating the heating chamber with a small amount of steam for the first time, wherein the amount of the steam is 1/3 after 1 hour, 1/3 of the steam is supplied after another 1 hour, and the steam is completely supplied after another 1 hour, based on the condition that the pressure of the heating chamber is not raised.
10. The method according to claim 8, characterized in that before crystallization of each effect liquid, the salt foot is drained once to remove impurities precipitated from each effect.
CN202111306886.9A 2021-11-05 2021-11-05 Preparation method of ecological well mineral salt Pending CN113979451A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111306886.9A CN113979451A (en) 2021-11-05 2021-11-05 Preparation method of ecological well mineral salt

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111306886.9A CN113979451A (en) 2021-11-05 2021-11-05 Preparation method of ecological well mineral salt

Publications (1)

Publication Number Publication Date
CN113979451A true CN113979451A (en) 2022-01-28

Family

ID=79746785

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111306886.9A Pending CN113979451A (en) 2021-11-05 2021-11-05 Preparation method of ecological well mineral salt

Country Status (1)

Country Link
CN (1) CN113979451A (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR341355A (en) * 1904-02-08 1904-08-06 Solvay Et Cie Soc Methods of manufacturing fillers for various uses
TW201420505A (en) * 2012-11-27 2014-06-01 Ailia Innovative Company Ltd Hong Kong Purification reagents for molten salts and the method of in-situ purification
CN104605307A (en) * 2015-02-04 2015-05-13 中盐东兴盐化股份有限公司 Method for preparing original ecology edible salt
CN111762800A (en) * 2020-05-19 2020-10-13 昆明理工大学 Method and system for preparing large-particle ice crystal salt
CN112679021A (en) * 2020-12-25 2021-04-20 儋州市中等职业技术学校 Method for preparing salt from seawater

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR341355A (en) * 1904-02-08 1904-08-06 Solvay Et Cie Soc Methods of manufacturing fillers for various uses
TW201420505A (en) * 2012-11-27 2014-06-01 Ailia Innovative Company Ltd Hong Kong Purification reagents for molten salts and the method of in-situ purification
CN104605307A (en) * 2015-02-04 2015-05-13 中盐东兴盐化股份有限公司 Method for preparing original ecology edible salt
CN111762800A (en) * 2020-05-19 2020-10-13 昆明理工大学 Method and system for preparing large-particle ice crystal salt
CN112679021A (en) * 2020-12-25 2021-04-20 儋州市中等职业技术学校 Method for preparing salt from seawater

Similar Documents

Publication Publication Date Title
CN106365181B (en) It is a kind of to utilize the method for preparing battery-level lithium carbonate containing higher impurity richness lithium solution
CN111960445B (en) Method for preparing battery-grade lithium carbonate by using lithium sulfate coarse ore and recycling by-products
CN107934996A (en) A kind of technique using triamine End gas production sodium bicarbonate and ammonium chloride
CN102491373B (en) Method for producing potassium chloride, sodium chloride and magnesium sheet from bittern extracted from carnallite mine
CN108275703B (en) Process for preparing lithium carbonate and potassium salt by using lithium-containing nanofiltration produced water
CN110699756B (en) Method for preparing alpha-type gypsum whisker by using ammonia-soda waste liquid
CN104071811A (en) Process for extracting lithium salt from spodumene by adopting sulfuric acid pressure boiling method
CN101683997A (en) Method for producing calcium chloride dihydrate
CN101591030A (en) The co-production of sodium-chlor, sal epsom, Repone K
CN112158865A (en) Method for recycling lithium element in lithium precipitation mother liquor
CN115893449B (en) Method for producing electronic grade sodium fluoride by using industrial grade sodium-alkali mixed solution
CN114906864A (en) Method for extracting lithium from high-calcium chloride type salt lake brine
CN101565189A (en) Method for preparing sodium chloride and potassium chloride by using brine
CN103818935A (en) Method for separating potassium oxide from potassium-containing sodium aluminate solution
CN101837998B (en) Method for evaporating, concentrating and crystallizing solution of aluminum chloride
CN115650256A (en) Industrial potassium chloride purification process and production system
CN102921553B (en) Method for flotation of lithium potassium sulfate in mixture of lithium potassium sulfate and sodium chloride
CN111153474A (en) Stevioside extraction flocculant and extraction process thereof
CN100562493C (en) Hot method is handled alkali-making mother solution, is produced the ammonium chloride industrialization technology
CN113979451A (en) Preparation method of ecological well mineral salt
WO2021073199A1 (en) Continuous production method for hydroxyethylene diphosphonic acid crystals
CN110923452A (en) Process for recovering potassium and sodium salts from lithium-precipitated liquid of lepidolite by using ethanol
CN1341557A (en) Joint production process of salt and salt-cake
CN102120592B (en) Method for extracting lithium carbonate by flotation of mixed salt of NaCl and lithium carbonate
CN115010152A (en) Lithium carbonate purification production process

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination