CN113753920B - Preparation method of low sodium salt - Google Patents
Preparation method of low sodium salt Download PDFInfo
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- CN113753920B CN113753920B CN202111244185.7A CN202111244185A CN113753920B CN 113753920 B CN113753920 B CN 113753920B CN 202111244185 A CN202111244185 A CN 202111244185A CN 113753920 B CN113753920 B CN 113753920B
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- mother liquor
- sodium salt
- carnallite
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
- C01D3/06—Preparation by working up brines; seawater or spent lyes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/22—Preparation in the form of granules, pieces, or other shaped products
- C01D3/24—Influencing the crystallisation process
Abstract
The invention discloses a preparation method of low sodium salt. The preparation method comprises the following steps: decomposing carnallite to obtain a first mother liquor and a sylvite solid; mixing the sylvite solids with fresh water to form a second mother liquor; and mixing the second mother solution with old brine for reaction and crystallization to obtain low sodium salt. The preparation method provided by the invention has the advantages of simple process flow, low energy consumption, low cost and environmental protection; the prepared low sodium salt product meets the standard requirements of low sodium salt QB/T2019-2020, has high purity and controllable particle size, and has stronger market competitiveness.
Description
Technical Field
The invention belongs to the technical field of inorganic salt industry, relates to a preparation method of low sodium salt, and in particular relates to a method for preparing low sodium salt by adding halogen and crystallizing.
Background
The habit of high sodium diet makes hypertension one of important diseases affecting body health, and low sodium salt is one of safe and effective measures for preventing diseases such as hypertension and the like.
The low sodium salt production technology has short development time in China, and the current effective production technology comprises a direct mixing method, a seawater or brine evaporation method, a saline soil plant leaching method and the like. The blending method needs food-grade additives, chemical purification has chemical pollution, and the cost is high, so that the cost of low sodium salt is generally high. Along with the pollution of different degrees in the sea area, the sea water is used for preparing the low sodium salt, so that the quality of the food-grade sea salt product can not be ensured. The saline soil plant leaching method is limited by regional resource distribution, and meanwhile, the extraction process is high in temperature and long in time, and the production cost is greatly increased.
The Qinghai province Qaidam region contains abundant sodium and potassium resources and has huge potential economic value. Aiming at preparing low sodium salt from salt lake resources, the patent CN201710109056.4 provides a preparation method for preparing a low sodium salt product meeting the requirements by adjusting the salt precipitation proportion in the natural evaporation process of chloride type salt lake brine; in patent CN201810726693.0, depending on sulfate type salt lake brine, sulfate radical is removed by utilizing climate conditions in a Qaidam region in winter, and a low-sodium salt product is prepared by natural evaporation; however, the two processes respectively need natural evaporation and freezing sulfate removal processes for preparing low sodium salt aiming at chloride type and sulfate type salt lake brine, the temperature is relatively strict, the particle size of the prepared low sodium salt product is uncontrollable, and the impurity removal process is needed for meeting the product requirements. Therefore, how to provide a low-sodium salt preparation method with simple process, low energy consumption and green color is a problem to be solved urgently.
Disclosure of Invention
The invention mainly aims to provide a preparation method of low sodium salt, which aims to overcome the defects of the prior art.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a preparation method of low sodium salt, which comprises the following steps:
decomposing carnallite to obtain a first mother liquor and a sylvite solid;
mixing the sylvite solids with fresh water to form a second mother liquor;
and mixing the second mother solution with a magnesium source for reaction and crystallization to obtain low sodium salt.
In some more specific embodiments, the method of making comprises: and mixing carnallite with fresh water, decomposing and filtering to obtain the first mother liquor and sylvite solid, wherein the mass ratio of the carnallite to the fresh water is 1:0.9-1.2.
In some more specific embodiments, the method of making comprises: and mixing the sylvite solid, naCl and fresh water to form the second mother liquor, wherein the mass ratio of the sylvite solid to the NaCl is 1:0-1.4.
In some more specific embodiments, the method of making comprises: and placing carnallite saturated mother liquor into a crystallization device, then adding the second mother liquor and a magnesium source into the carnallite saturated mother liquor in a two-way manner by adopting a peristaltic pump, performing reactive crystallization at room temperature, and then washing, filtering and drying to obtain the low sodium salt.
Compared with the prior art, the invention has the beneficial effects that:
(1) The preparation method provided by the invention has the advantages of simple process flow, low energy consumption, low cost and environmental protection; the whole reaction process is carried out in a liquid phase, which is very beneficial to directly removing impurities such as sediment, suspended matters, water insoluble matters and the like in the process; the product quality can be ensured without additional impurity removal devices in the whole process;
(2) The invention can realize recycling of byproduct old brine of potassium extraction, and the carnallite decomposition mother liquor can be continuously used for producing carnallite ore by evaporation, thus realizing the recycling of the mother liquor;
(3) The low sodium salt product prepared by the invention meets the standard requirements of low sodium salt QB/T2019-2020, has high purity and controllable particle size, and has stronger market competitiveness.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments described in the present invention, and other drawings may be obtained according to the drawings without inventive effort to those skilled in the art.
FIG. 1 is a flow chart of the preparation of low sodium salt in an exemplary embodiment of the present invention;
fig. 2 is a theoretical calculation of low sodium salt in an exemplary embodiment of the invention.
Description of the embodiments
In view of the defects of the prior art, the inventor of the present invention has provided the technical proposal of the present invention through long-term research and a great deal of practice, the present invention relies on the salt lake to produce by-product old brine (or MgCl) 2 ·6H 2 O、MgCl 2 ) And directly preparing a high-purity low-sodium salt crude product from carnallite and fresh water resources by a halogen adding method, and then filtering and drying to directly obtain the low-sodium salt which is 20% -35% in terms of KCl content, and has the advantages of high purity, controllable particle size, greenness and no pollution. The whole production process is simple in process, does not have any chemical addition, and completely meets the requirements of green original ecological products.
The following description of the present invention will be made clearly and fully, and it is apparent that the embodiments described are some, but not all, of the embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Specifically, as one aspect of the technical scheme of the invention, the preparation method of the low sodium salt comprises the following steps:
decomposing carnallite to obtain a first mother liquor and a sylvite solid;
mixing the sylvite solids with fresh water to form a second mother liquor;
and mixing the second mother solution with a magnesium source for reaction and crystallization to obtain low sodium salt.
In some preferred embodiments, the preparation method specifically comprises: and mixing carnallite with fresh water, decomposing and filtering to obtain the first mother liquor and sylvite solid, wherein the mass ratio of the carnallite to the fresh water is 1:0.9-1.2.
In some preferred embodiments, the chemical composition of the carnallite comprises: k (K) + 7.0~12.2wt%、Mg 2+ 6.9~8.6wt%、Cl - 36.0~46.2wt%、Na + 0~12.8wt%、H 2 O 27.1~43.3wt%。
And/or recovering the first mother liquor for tedding treatment to obtain carnallite.
And/or the chemical composition of the sylvite solid comprises: na (Na) + 7.30~9.10wt%、K + 4.51~5.91wt%、Mg 2+ 0.51~0.77wt%、Cl - 17.99~19.80wt%。
In some preferred embodiments, the preparation method specifically comprises: and mixing the sylvite solid, naCl and fresh water to form the second mother liquor, wherein the mass ratio of the sylvite solid to the NaCl is 1:0-1.4.
In some preferred embodiments, the mass ratio of the sylvite solids to the fresh water is 1 (2.2-2.6).
In some preferred embodiments, the chemical components of the second mother liquor include: na (Na) + 7.1~10wt%、K + 3.6~5.3wt%、Mg 2+ 0.8~0.93wt%、Cl - 18.2~21.4wt%、H 2 O 64~68.8wt%。
In some preferred embodiments, the preparation method specifically comprises: and placing carnallite saturated mother liquor into a crystallization device, then adding the second mother liquor and a magnesium source into the carnallite saturated mother liquor in a two-way manner by adopting a peristaltic pump, performing reactive crystallization at room temperature, and then washing, filtering and drying to obtain the low sodium salt.
Further, the chemical components of the carnallite saturated mother liquor comprise: na (Na) + 0.6~0.8wt%、K + 1.6~1.8wt%、Mg 2+ 5.9~6.6wt%、Cl - 21.4~22.3wt%、H 2 O 68.5~69.8wt%。
Further, the magnesium source comprises old brine and MgCl 2 ·6H 2 O、MgCl 2 Any one or a combination of two or more of them, and is not limited thereto.
Further, the chemical components of the old brine include: na (Na) + 0.39~1.86wt%、K + 0.01~0.1wt%、Mg 2+ 8.3~9.2wt%、Cl - 24.3~27.2wt%、H 2 O 62.6~63.3wt%。
Further, the time for adding the second mother solution and the magnesium source to the carnallite saturated mother solution in a two-way manner is 30 min-5 h.
Further, the mass ratio of the second mother liquor to the magnesium source is 1: (0.3 to 2.9).
Further, the content of KCl in the low sodium salt is 20-35 wt%.
In some more preferred embodiments, the method of preparing the low sodium salt comprises:
(1) Carnallite is decomposed and filtered by adding fresh water to obtain mother liquor L1 (also the first mother liquor) and sylvite solid S1, wherein the chemical components of S1 comprise: na (Na) + 7.30~9.10wt%、K + 4.51~5.91wt%、Mg 2+ 0.51~0.77wt%、Cl - 17.99~19.80wt%；
(2) S1 (proper addition of very little NaCl regulatory system Na + Content) and fresh water according to a mass ratio of 1: (2.2-2.6) preparing mother liquor L2 (also the second mother liquor);
(3) The mother liquor is saturated with carnallite in a crystallizer (the chemical components of the carnallite saturated mother liquor include Na + 0.6~0.8%、K + 1.6~1.8%、Mg 2+ 5.9~6.6%、Cl - 21.4~22.3%、H 2 O68.5-69.8%), as a base solution, and simultaneously, dropwise adding L2 and old brine in a peristaltic pump in a bidirectional manner, controlling different feeding times to obtain low sodium salt crude products with different granularities, and washing, filtering and drying to obtain the low sodium salt product meeting the low sodium salt composition requirement.
Preferably, the magnesium source is MgCl 2 ·6H 2 O or MgCl 2 。
The preparation flow chart and theoretical calculation of the low sodium salt in the invention are shown in fig. 1 and 2 respectively.
The invention relates to a method for preparing low sodium salt by taking byproduct old brine, carnallite and fresh water in salt lake as raw materials, which is characterized in that a low sodium salt crude product can be obtained only by adding brine at normal temperature, and then a green low sodium salt product with high quality and controllable particle size (20% -35% of KCl content) can be directly obtained by washing, filtering and drying.
The technical scheme of the present invention is further described in detail below with reference to several preferred embodiments and the accompanying drawings, and the embodiments are implemented on the premise of the technical scheme of the present invention, and detailed implementation manners and specific operation processes are given, but the protection scope of the present invention is not limited to the following embodiments.
The experimental materials used in the examples described below, unless otherwise specified, were all commercially available from conventional biochemicals.
Example 1
Decomposing and filtering carnallite by adding fresh water to obtain mother liquor L1 and sylvite solid S1;
mixing solid S1 with fresh water according to a mass ratio of 1:2.2 dissolving to obtain mother liquor L2, wherein the chemical composition of S1 is as follows: na (Na) + 7.30wt%、K + 5.91wt%、Mg 2+ 0.56wt%、Cl - 17.99wt%; the mother liquor at point E in FIG. 2 (chemical composition of mother liquor at point E: na + 0.6~0.8wt%、K + 1.6~1.8wt%、Mg 2+ 5.9~6.6wt%、Cl - 21.4~22.3wt%、H 2 O68.5-69.8wt% is 15L of base liquid, and 5.20kg of L2 and 5.90kg of old brine (Na + 0.33wt%、K + 0.03wt%、Mg 2+ 8.34wt%、Cl - 24.85wt percent) and simultaneously adding the mixture into a crystallizer at one time, filtering after the reaction is finished for 30min to obtain a low sodium salt product with the KCl content of 22.88wt percent, and sieving the low sodium salt product to obtain the low sodium salt product with the particle size distribution d of more than 180 mu m of 9.02%, the particle size distribution d of 150 mu m of less than 180 mu m of 7.21%, the particle size d of 125 mu m of less than 150 mu m of 82.1%.
Example 2
Decomposing and filtering carnallite by adding fresh water to obtain mother liquor L1 and sylvite solid S1;
mixing solid S1 with fresh water according to a mass ratio of 1:2.6 dissolving to obtain mother liquor L2, wherein the chemical composition of S1 is as follows: na (Na) + 8.00wt%、K + 5.78wt%、Mg 2+ 0.51wt%、Cl - 19.12wt%; adding the E point mother liquor in the graph 1 as base liquor 15L into a 15L crystallizer, respectively taking 8.90kg L2 and 9.81kg of old brine at the same time, adopting a bidirectional dropping method, controlling the feeding speed by a peristaltic pump, adding into the crystallizer, reacting for 30min, filtering to obtain a low sodium salt product with KCl content of 26.81wt%, and sieving to obtain a low sodium salt product with particle size distribution d of more than 180 μm of 74.36wt%, d of 150 μm < 180 μm of 3.59wt%, d of 125 μm < 150 μm of 7.76wt%.
Example 3
Decomposing and filtering carnallite by adding fresh water to obtain mother liquor L1 and sylvite solid S1;
mixing solid S1 with fresh water according to a mass ratio of 1:2.3 dissolving to obtain mother liquor L2, wherein the chemical composition of S1 is as follows: na (Na) + 9.10wt%、K + 4.73wt%、Mg 2+ 0.57wt%、Cl - 19.80wt%; adding the E point mother liquor in the graph 1 as base liquor 15L into a 15L crystallizer, respectively taking 8.99kg L2 and 9.93kg of old brine at the same time, adopting a bidirectional dropping method, controlling the feeding speed by a peristaltic pump, adding into the crystallizer, reacting for 30min, filtering to obtain a low sodium salt product with KCl content of 32.36wt%, and sieving to obtain a low sodium salt product with particle size distribution d of more than 180 μm of 78.84wt%, d of 150 μm of less than 180 μm of 2.24wt%, d of 125 μm of less than 150 μm of 8.67wt%.
Example 4
Decomposing and filtering carnallite by adding fresh water to obtain mother liquor L1 and sylvite solid S1;
mixing solid S1 with fresh water according to a mass ratio of 1:2.5 dissolving to obtain mother liquor L2, wherein the chemical composition of S1 is as follows: na (Na) + 8.36wt%、K + 4.51wt%、Mg 2+ 0.77wt%、Cl - 19.03wt%; adding the E point mother liquor in the graph 1 as base liquor 15L into a 15L crystallizer, respectively taking 8.99kg L2 and 9.93kg of old brine at the same time, adopting a bidirectional dropping method, controlling the feeding speed by a peristaltic pump, adding into the crystallizer, reacting for 30min, filtering to obtain a low sodium salt product with KCl content of 31.56wt%, and sieving to obtain a low sodium salt product with particle size distribution d of more than 180 μm of 83.97wt%, d of 150 μm of less than 180 μm of 1.94wt%, d of 125 μm of less than 150 μm of 5.58wt%.
Example 5
Decomposing and filtering carnallite by adding fresh water to obtain mother liquor L1 and sylvite solid S1;
mixing solid S1 with fresh water according to a mass ratio of 1:2.5 dissolving to obtain mother liquor L2, wherein the chemical composition of S1 is as follows: na (Na) + 8.36wt%、K + 4.51wt%、Mg 2+ 0.77wt%、Cl - 19.03wt%; adding the mother liquor at E point in FIG. 1 as base solution 15L into 15L crystallizer, respectively taking 8.99kg L2 and 7.00kg MgCl simultaneously 2 ·6H 2 O, adopting a bidirectional dropping method, controlling the feeding speed by a peristaltic pump for 5h, adding the mixture into a crystallizer, filtering after the reaction is finished for 30min to obtain a low sodium salt product with the KCl content of 31.56wt%, and screening to obtain a low sodium salt product with the particle size distribution d of more than 180 mu m of 83.97wt%, the d of 150 mu m of less than 180 mu m of 1.94wt% and the d of 125 mu m of less than 150 mu m of 5.58wt%.
Example 6
Decomposing and filtering carnallite by adding fresh water to obtain mother liquor L1 and sylvite solid S1;
mixing solid S1 with fresh water according to a mass ratio of 1:2.5 dissolving to obtain mother liquor L2, wherein the chemical composition of S1 is as follows: na (Na) + 8.36wt%、K + 4.51wt%、Mg 2+ 0.77wt%、Cl - 19.03wt%; adding the mother liquor at E point in FIG. 1 as base solution 15L into 15L crystallizer, respectively taking 8.99kg L2 and 3.28kg MgCl simultaneously 2 The method comprises the steps of adopting a bidirectional dropping method, controlling the feeding speed by a peristaltic pump for 5h, adding the mixture into a crystallizer, filtering after the reaction is finished for 30min, obtaining a low sodium salt product with the KCl content of 31.56wt%, and screening the low sodium salt product to obtain the low sodium salt product with the KCl content of 83.97wt% when the particle size distribution d is more than 180 mu m, 1.94wt% when the particle size d is more than 150 mu m and less than 180 mu m, and 5.58wt% when the particle size d is more than 125 mu m and less than 150 mu m.
In addition, the inventors have conducted experiments with other materials, process operations, and process conditions as described in this specification with reference to the foregoing examples, and have all obtained desirable results.
It should be understood that the technical solution of the present invention is not limited to the above specific embodiments, and all technical modifications made according to the technical solution of the present invention without departing from the spirit of the present invention and the scope of the claims are within the scope of the present invention.
Claims (4)
1. A method for preparing a low sodium salt, comprising:
mixing carnallite and fresh water at room temperature for decomposition and filtration to obtain a first mother solution and a sylvite solid; wherein the mass ratio of carnallite to fresh water is 1:0.9-1.2; the chemical components of the carnallite comprise: k (K) + 7.0~12.2wt%、Mg 2+ 6.9~8.6wt%、Cl - 36.0~46.2wt%、Na + 0~12.8wt%、H 2 27.1-43.3wt% of O; the chemical components of the sylvite solid comprise: na (Na) + 7.30~9.10wt%、K + 4.51~5.91wt%、Mg 2+ 0.51~0.77wt%、Cl - 17.99~19.80wt%；
Mixing the sylvite solids, naCl and fresh water to form a second mother liquor; wherein the sylvite solids are with NaClThe mass ratio is 1:0-1.4; the mass ratio of the sylvite solid to the fresh water is 1 (2.2-2.6); the chemical components of the second mother liquor comprise: na (Na) + 7.1~10wt%、K + 3.6~5.3wt%、Mg 2+ 0.8~0.93wt%、Cl - 18.2~21.4wt%、H 2 O 64~68.8wt%；
Placing carnallite saturated mother liquor into a crystallization device, then adopting a peristaltic pump to bidirectionally add the second mother liquor and a magnesium source into the carnallite saturated mother liquor, performing reaction crystallization at room temperature, and then washing, filtering and drying to obtain low sodium salt; wherein, the chemical components of the carnallite saturated mother liquor comprise: na (Na) + 0.6~0.8wt%、K + 1.6~1.8wt%、Mg 2+ 5.9~6.6wt%、Cl - 21.4~22.3wt%、H 2 68.5-69.8wt% of O; the magnesium source is selected from old brine and MgCl 2 ·6H 2 O、MgCl 2 Any one or a combination of two or more of them; the chemical components of the old brine comprise: na (Na) + 0.39~1.86wt%、K + 0.01~0.1wt%、Mg 2+ 8.3~9.2wt%、Cl - 24.3~27.2wt%、H 2 O 62.6~63.3wt%；
Wherein the content of KCl in the low sodium salt is 20-35wt%.
2. The method according to claim 1, wherein the first mother liquor is recovered and subjected to tedding treatment to obtain carnallite.
3. The method of manufacturing according to claim 1, characterized in that: and the time for adding the second mother solution and the magnesium source into the carnallite saturated mother solution in a two-way manner is 30 min-5 h.
4. The method of manufacturing according to claim 1, characterized in that: the mass ratio of the second mother liquor to the magnesium source is 1: (0.3 to 2.9).
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| CN101905895A (en) * | 2010-08-10 | 2010-12-08 | 山西大学 | Method for producing potassium chloride by using sylvite as raw material |
| CN102491372B (en) * | 2011-11-30 | 2013-08-14 | 化工部长沙设计研究院 | Method of producing potassium chloride from reverse flotation tailings of carnallite |
| CN102491373B (en) * | 2011-12-22 | 2013-08-14 | 化工部长沙设计研究院 | Method for producing potassium chloride, sodium chloride and magnesium sheet from bittern extracted from carnallite mine |
| CN105668592B (en) * | 2016-04-12 | 2018-04-03 | 浙江丛晟食品科技股份有限公司 | The production method of low sodium high-purity potassium chloride |
| CN109467107A (en) * | 2018-12-25 | 2019-03-15 | 青海盐湖工业股份有限公司 | A kind of production method of sylvite |
| CN111533138B (en) * | 2020-05-06 | 2022-08-26 | 中国科学院青海盐湖研究所 | Method for preparing potassium chloride by utilizing carnallite |
| CN112340753B (en) * | 2020-11-23 | 2022-11-08 | 青海盐湖工业股份有限公司 | Method and system for recycling potassium chloride |
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