CN114403416A - Low-sodium salt with spherical structure and spray preparation method thereof - Google Patents

Low-sodium salt with spherical structure and spray preparation method thereof Download PDF

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CN114403416A
CN114403416A CN202210122581.0A CN202210122581A CN114403416A CN 114403416 A CN114403416 A CN 114403416A CN 202210122581 A CN202210122581 A CN 202210122581A CN 114403416 A CN114403416 A CN 114403416A
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sodium salt
low
chloride
spherical
salt
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CN114403416B (en
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邱常义
熊泽华
于建国
孙玉柱
罗孟杰
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Jiangxi Fu Da Salt Product Co ltd
East China University of Science and Technology
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Jiangxi Fu Da Salt Product Co ltd
East China University of Science and Technology
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    • 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
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    • 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
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    • 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
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    • 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
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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Abstract

The invention belongs to the technical field of chemical engineering spray drying, and particularly relates to a low sodium salt with a spherical structure and a spray preparation method thereof, wherein the low sodium salt comprises 65-80 wt% of sodium chloride, 20-35 wt% of potassium chloride and 0.003-1.5 wt% of micronutrients; the shape of the solid particles of the low sodium salt is spherical aggregate particles, sodium chloride and potassium chloride are uniformly embedded in each particle, and micronutrients are uniformly dispersed on the surface or the periphery of the particles. The low sodium salt is spherical aggregate, the surface of the granule is compact, the sodium chloride and the potassium chloride are uniformly distributed and embedded in the same spherical granule, and the micronutrients are uniformly dispersed on the surface or around the spherical granule; the product prepared by the method has the advantages of superfine particles, uniform particle size distribution, small average particle size, high sphericity, good fluidity, better anti-caking property, simple preparation process and easy industrial production.

Description

Low-sodium salt with spherical structure and spray preparation method thereof
Technical Field
The invention belongs to the technical field of chemical engineering spray drying, and particularly relates to a low-sodium salt with a spherical structure and a spray preparation method thereof.
Background
The world health organization proposed a salt reduction action to countries in the world, and large cities such as Beijing and Shanghai have begun to promote the consumption of low-sodium salt. At present, 85% of deaths of residents in China are caused by chronic diseases, and long-term excessive salt intake is one of the main reasons for inducing various diseases such as hypertension, cardiovascular and cerebrovascular diseases, cerebral apoplexy and the like. The low-sodium salt is edible salt which is prepared by processing edible sodium chloride, edible potassium chloride or edible magnesium sulfate (edible magnesium chloride) serving as main raw materials according to a scientific and reasonable proportion. Compared with common salt, the low-sodium salt of the low-sodium salt mainly replaces sodium ions with potassium ions, so that the content of sodium is reduced, the morbidity of hypertension caused by high-sodium intake factors is reduced, and potassium, magnesium and other nutrient elements are increased, thereby being more beneficial to the balance of various nutrient components. The low-sodium salt is popularized in some big cities and economically developed areas, and with the improvement of living conditions and the emphasis of health ideas of people, the low-sodium salt product has wide development prospect and market development as the development direction of future seasonings.
The low-sodium salt particles are used as carriers, and are added with various nutrient substances such as minerals, vitamins, amino acids and the like, so that the potassium-reducing salt has a potassium-reducing effect, develops various nutritional functions, has higher nutritional value than the common low-sodium salt, and becomes a development trend of high-end salt. The salt is an indispensable seasoning for daily diet, so compared with special taking of nutritional supplements, the mode of adding nutrients on the salt for intake is simpler and more efficient, the complex operation brought by special taking of various nutritional supplements is avoided, and the purpose of long-term stable intake of nutrients is easier to achieve.
At present, the preparation method of low sodium salt at home and abroad mainly comprises a direct mixing method, a seawater or brine evaporation method and a saline soil plant leaching method. (1) Direct mixing method: edible sodium chloride, edible potassium salt, magnesium salt and other raw materials are uniformly mixed by adopting a mechanical mixing process according to a formula proportion. Since the taste of the salt is slightly bitter and easy to cake after adding potassium, magnesium, etc., additives such as organic acids for masking bitterness and anticaking agents such as potassium ferrocyanide, silicon dioxide, magnesium carbonate, etc. for preventing caking are often added to the low-sodium salt to improve the taste and fluidity of the low-sodium salt. The method mainly has the problems that the low-sodium salt is prepared by mechanical mixing, so that the sodium chloride and the potassium chloride cannot be uniformly mixed, particularly, the potassium chloride is not uniformly distributed, and the taste of the low-sodium salt product is reduced; meanwhile, the food additive is added into the low-sodium salt product for masking bitterness or preventing agglomeration, so that the requirements of natural green products are not met, and the food additive is expensive, so that the manufacturing cost of the low-sodium salt is increased. (2) Seawater or brine evaporation: the method adopts a salt drying process, namely seawater or brine is used as a raw material, natural evaporation and concentration are carried out on the raw material to obtain saturated brine, and then natural evaporation is carried out under sunlight to directly prepare low-sodium salt; the solar salt drying process generally selects a crystallization tank as evaporation and crystallization equipment, obtains a low-sodium salt product through brine tank filling, natural evaporation, salt spraying, crystal growth and product harvesting, and regulates and controls the quality of the low-sodium salt product by controlling the brine crystallization termination concentration. However, when seawater or brine is used for natural evaporation, because environmental pollution is serious in recent years, various sea areas are polluted to different degrees, harmful impurities such as flotation reagents and the like are contained in the brine, and if the low-sodium salt product is produced by direct evaporation and crystallization without deep impurity removal, the product quality of the low-sodium salt cannot be guaranteed; the natural evaporation method is limited by the change of climate, adopts the traditional evaporation equipment such as a crystallization tank and the like, has long evaporation time and low efficiency, and the granularity of the product obtained by crystallization is not uniform. (3) Saline soil plant leaching method: the low sodium salt is prepared by using saline soil plants, wherein some saline soil plants in some regions contain sodium chloride, potassium chloride, magnesium chloride, amino acid and the like. The method is mainly limited by regional resource distribution, the extraction process is high in temperature and long in time, and the obtained low-sodium salt product is low in amino acid content.
At present, a few scholars propose a technical method for preparing a low-sodium salt product by a spray drying method, the prepared low-sodium salt product has small granularity and uniform distribution of potassium and sodium components, but the particle morphology is still mostly cubic, and the contact area among particles is larger. Considering that the molecular structure of nutrient substances such as inorganic salt minerals, amino acids, vitamins and the like is different from sodium chloride greatly, crystal particles in the forms of eutectic crystals and the like are difficult to form and only can adopt a physical coating form, but the nutrient substances such as the vitamins, the amino acids and the like are easy to adhere to the surfaces of cubic salt particles to cause the negative coalescence of solid particles, so that the salt is easy to agglomerate seriously in the spray granulation process, the particle size difference is generated, the particle shape is irregular, and the nutrient substances are finally distributed unevenly. Due to the difficulties, the deep development and diversified popularization of the high-end salt variety of the low-sodium nutritive salt are limited to a great extent.
Therefore, the improvement of the spray drying technology is needed to prepare a low-sodium salt high-end product capable of uniformly attaching mineral substances, vitamins and amino acid nutrients, the uniform particle size, regular particle shape and good sphericity of the product are realized, the fluidity of the product is improved, the caking resistance is good, the preparation process is simple, and the industrial production is easy to realize.
Disclosure of Invention
The invention aims to overcome the defects of uneven distribution of potassium chloride and nutrient substances, large product granularity difference, poor fluidity, easy caking and the like in the prior low-sodium salt preparation technology and provide a low-sodium salt with a spherical structure and a spray preparation method thereof, wherein the low-sodium salt is characterized in that the main components comprise 65-80% of sodium chloride, 20-35% of potassium chloride and 0.003-1.5% of micronutrient substances; the shape of the solid particles is spherical aggregate, the surface of the particles is compact, sodium chloride and potassium chloride are uniformly distributed and embedded in the same spherical particle, and micronutrients are uniformly dispersed on the surface or around the spherical particle; the product prepared by the method has superfine particles, uniform particle size distribution, average particle size of 10-200 mu m, sphericity of more than 90 percent, good fluidity and better anti-caking property.
The invention provides a low sodium salt with a spherical structure, which comprises the following main components of 65-80 wt% of sodium chloride, 20-35 wt% of potassium chloride and 0.003-1.5 wt% of micronutrients;
the shape of the solid particles of the low sodium salt is spherical aggregate particles, the surfaces of the particles are compact, the sodium chloride and the potassium chloride are uniformly embedded in each particle, and the micronutrients are uniformly dispersed on the surfaces of the particles or on the periphery of the particles.
Preferably, in the above technical solution, the low sodium salt particles have an average particle size of 10 to 200 μm.
Preferably, in the above technical solution, the sphericity of the low sodium salt is greater than 90%.
The invention also provides a spray preparation method of the low sodium salt with the spherical structure, which comprises the following specific steps:
s1, crushing a main raw material, dissolving the main raw material in a certain amount of water, and carrying out solid-liquid separation to obtain insoluble substances to obtain a filtrate;
s2, separating trace impurity ions from the filtrate obtained in the step S1 by adopting a nanofiltration separation technology to obtain a refined sodium chloride solution with the mass fraction of NaCl lower than 25% and the content of the impurity ions lower than 0.5%;
s3, adding food-grade potassium chloride with a certain mass into the sodium chloride solution obtained in the S2 to prepare an unsaturated solution at normal temperature;
s4, adding nutrient substances into the unsaturated solution obtained in the step S3, and carrying out suspension stirring for 0.5-3h at normal temperature at the stirring speed of 200-600 r/min;
s5, carrying out ion spray drying on the suspension obtained in the step S4 to prepare the micron-sized superfine spherical low-sodium salt.
The invention adopts spray drying to prepare the superfine low-sodium salt product with uniform granularity, good sphericity and uniform distribution of potassium and sodium components, and the key point is to ensure the atomization effect of liquid drops in a spray drying tower. When the suspension solution is fed to the atomizing disk rotating at high speed, the solution spreads as a thin film on the rotating surface due to centrifugal force and moves with increasing speed to the edge of the disk, and when it leaves the edge of the disk, the liquid is atomized. According to the invention, by optimizing key operation parameters such as liquid inlet amount, atomizer type and rotating speed in the spray drying process, the solution is enabled to be subjected to drop-shaped atomization in the spray tower, the proper size of the fog drops is generated, and the uniformity of the fog drops is improved, so that the fog drops are rapidly contacted and dried with hot air in the falling process, and finally spherical product particles are generated.
Preferably, in the technical scheme S1, the main raw material is one or more of natural crystalline rock salt ore, natural argillaceous rock salt ore, natural sylvine salt ore, and food-grade sodium chloride.
The raw materials for preparing the low-sodium salt are wide, and the low-sodium salt is one or more of natural crystalline halite ore, natural argillaceous halite ore, natural sylvine ore and food-grade sodium chloride. Wherein the main chemical components of the natural crystalline halite ore comprise 90-99% of NaCl, 0-0.01% of KCl and 0-0.05% of Na2SO4、0-0.5%CaSO40.5-7.4% of other soluble salt and 0.5-2.0% of water insoluble substance; the main chemical components of the natural argillaceous halite ore comprise 65-75% of NaCl, 0-0.1% of KCl and 4-5% of Na2SO4、5-6%CaSO41-4% of other soluble salt and 15-20% of water insoluble substance; the main chemical components of the natural sylvine ore are 55-65% of NaCl, 30-35% of KCl and 0.5-1.0% of Na2SO4、2-3%MgCl22.5-6.0% water insoluble matter; the main chemical components of the food-grade sodium chloride are 98-99.8% of NaCl and 0.1-0.5% of Na2SO40.1-1.5% of other impurities; the main chemical components of the food-grade potassium chloride are 97-99% of KCl, 0.5-1.0% of NaCl and 0.5-2.0% other impurities.
Preferably, in the above technical scheme, in S4, the nutrient substance is one or a combination of more than one of ferrous gluconate, ferrous citrate, calcium lactate, calcium gluconate, zinc lactate, zinc gluconate, potassium iodate, sodium selenite, vitamin a, vitamin D, vitamin E, lysine, phenylalanine, tryptophan, and glutamic acid at any ratio.
The low-sodium salt of the invention has wide nutrient components and is one or more of ferrous gluconate, ferrous citrate, calcium lactate, calcium gluconate, zinc lactate, zinc gluconate, potassium iodate, sodium selenite, vitamin A, vitamin D, vitamin E, lysine, phenylalanine, tryptophan and glutamic acid; there is no proportionality requirement for the various blends. Wherein, the addition amount of the ferrous gluconate and the ferrous citrate is 0.02 to 0.1 percent; the addition amount of calcium citrate, calcium lactate and calcium gluconate is 0.1-1.0%; the addition amount of zinc lactate and zinc gluconate is 0.01-0.05%; the addition amount of potassium iodate and sodium iodate is 0.005-0.01%; the addition amount of vitamin A, vitamin D and vitamin E is 0.15-1.5%; the addition amount of lysine, phenylalanine, tryptophan and glutamic acid is 0.1-0.5%.
Preferably, in the above technical solution S2, the process conditions of the nanofiltration separation technology are as follows: the membrane area is 0.24-1.0m2, the nanofiltration pressure is 0.5-3.0MPa, and the nanofiltration time is 0.5-3 h.
The nanofiltration separation technology in the technical scheme of the invention adopts the nanofiltration membrane to deeply remove trace impurities, utilizes the good separation capacity of the nanofiltration membrane, can quickly and efficiently remove high-valence ions such as sulfate radicals and the like in the sodium chloride solution, and can not introduce new impurities, the nanofiltration condition adopting the technical scheme can remove trace high-valence ion impurities in the sodium chloride raw material solution, and the removal rate can reach more than 99%.
Preferably, in the technical solution S3, the mass fraction of sodium chloride in the unsaturated solution is controlled to be 18.3-21.6% and the mass fraction of potassium chloride is controlled to be 5.4-9.8% by controlling the addition amount of potassium chloride.
Low as determined experimentally in combination with the product requirements of the inventionNaCl-KCl-H at 25 deg.C and 100 deg.C2And (3) a 0 ternary system phase diagram, establishing a crystallization route of spray drying low sodium salt, combining a proper composition range of a solid dry basis in a potassium chloride and sodium chloride co-crystallization area, and deducing proper initial compositions of sodium chloride and potassium chloride raw materials according to an evaporation ray, wherein the mass fraction of sodium chloride is 18.3-21.6%, and the mass fraction of potassium chloride is 5.4-9.8%, so as to prepare an unsaturated low sodium salt solution. According to the invention, the initial composition of sodium chloride and potassium chloride raw materials is obtained in advance according to the phase diagrams of the NaCl-KCl-H2O ternary systems at room temperature and high temperature, so that the precise control of the potassium and sodium components of the low-sodium salt product corresponding to the spray drying end point can be realized, the method is simple and efficient, and the test cost can be saved.
Preferably, in the technical solution S4, the addition amount of the nutrient is 0.005-1.5% of the total mass of the sodium chloride and the potassium chloride.
Preferably, in the above technical solution S5, during the spray centrifugal drying, the solution feeding pump speed is adjusted to 50-400mL/min, the atomizer rotation speed is 7500-.
Compared with the prior art, the method has the beneficial effects that:
1. the raw materials for preparing the low-sodium salt have wide sources and strong adaptability, can be natural ores such as crystalline halite ores, argillaceous halite ores and sylvite ores, can also be common salt products, and can be used as the raw materials for preparing the low-sodium salt products by spraying after the technological operations such as dissolution, solid-liquid separation, nanofiltration, potassium supplementation and the like.
2. In order to prepare the qualified low-sodium-salt product meeting the requirements of potassium and sodium components in the national standard (QB/T2019-2And an O ternary system phase diagram finds a proper potassium-sodium composition interval of the spray drying initial solution by regulating and controlling the water adding amount and the potassium chloride adding amount, and realizes the accurate control of the potassium-sodium component of the low-sodium salt product corresponding to the spray drying end point.
3. The nutrient substances added into the low sodium salt can realize single or compound nutrient function, and the added nutrient substances such as mineral substances such as calcium, iron, iodine and the like, vitamins, amino acids and the like can be uniformly distributed on the surfaces and the peripheries of sodium chloride and potassium chloride particles singly or compositely, so that the multi-variety and multi-nutrient function of the low sodium salt product is realized.
4. The low-sodium salt product prepared by the method has narrow and uniform particle size distribution and small average particle size; the product particles are spherical aggregates, so that the spherical granulation effect is achieved, and meanwhile, due to the fact that the direct contact area of the spherical particles is small, negative agglomeration of common cubic salt under the high viscosity of nutrient substances can be effectively avoided, particle bonding and agglomeration in the spray drying process are effectively reduced, and the product has good anti-caking property; the product particles have compact surfaces, and SEM-EDS measurement shows that potassium, sodium and chlorine elements are uniformly distributed and are uniformly embedded in the same spherical particle, so that sodium chloride and potassium chloride are uniformly distributed and embedded in the same spherical particle, and micronutrients are uniformly dispersed on the surfaces or around the spherical particle.
5. The invention adopts the spray centrifugal drying technology, controls various process parameters by ensuring the atomization effect of liquid drops in the spray drying tower, and prepares the high-end low-sodium salt which has uniform granularity, good sphericity, uniform distribution of potassium and sodium components and simultaneously adheres to nutrient substances, and the product has good fluidity and better caking resistance, and has simple preparation process and easy industrial production.
Drawings
FIG. 1 is a graph showing the particle size distribution of the low sodium salt product of the present invention;
FIG. 2 is a 100 μm scanning electron microscope image of the microscopic morphology of the spherical low-sodium salt product of the present invention;
FIG. 3 is a scanning electron microscope image of 10 μm of the microscopic morphology of the spherical low-sodium salt product of the present invention;
FIG. 4 is a 50 μm SEM-energy spectrum of the spherical low-sodium salt product of the present invention (where a is Na element distribution, b is K element distribution, and c is Cl element distribution).
Detailed Description
The technical features of the present invention described above and those described in detail below (as an embodiment) can be combined with each other to form a new or preferred technical solution, but the present invention is not limited to these embodiments, and the embodiments also do not limit the present invention in any way.
The experimental procedures in the following examples are conventional unless otherwise specified. The formulations according to the following examples are all commercially available products and are commercially available, unless otherwise specified.
The present invention is described in further detail below with reference to examples:
example 1
A spray preparation method of low sodium salt with a spherical structure comprises the following specific steps:
s1, crushing natural crystalline halite ores, dissolving the crushed natural crystalline halite ores in a certain amount of water, and carrying out solid-liquid separation to obtain insoluble substances to obtain filtrate;
s2, separating trace impurity ions from the filtrate obtained in the step S1 by adopting a nanofiltration separation technology to obtain a refined sodium chloride solution, and controlling the nanofiltration process condition to be that the membrane area is 0.24m2The nanofiltration pressure is 3.0MPa, and the nanofiltration time is 1 h;
s3, adding food-grade potassium chloride with a certain mass into the sodium chloride solution obtained in the S2 to prepare an unsaturated solution at normal temperature, wherein the mass fraction of sodium chloride in the unsaturated solution is controlled to be 18.3-21.6%, and the mass fraction of potassium chloride is controlled to be 5.4-9.8%;
s4, adding potassium iodate nutrient substances accounting for 0.005 percent of the total mass of the sodium chloride and the potassium chloride into the unsaturated solution obtained in the step S3, and carrying out suspension stirring for 1 hour at normal temperature, wherein the stirring speed is 400 r/min;
s5, carrying out ion spray drying on the suspension obtained in the step S4, controlling the solution feeding pump speed to be 200mL/min, the atomizer rotating speed to be 10000r/min, the air inlet temperature to be 200 ℃ and the air outlet temperature to be 100 ℃, and preparing micron-sized superfine spherical-structure low sodium salt, wherein the main components of the low sodium salt comprise 79.5% of sodium chloride, 20.4% of potassium chloride and 0.003% of nutrient iodine element; the particle size distribution of the product is uniform, and the average particle size is 42 mu m; the sphericity is 95%. Compared with common low-sodium salt, the product has the effect of supplementing iodine additionally.
Example 2
A spray preparation method of low sodium salt with a spherical structure comprises the following specific steps:
s1, crushing natural ore containing argillaceous halite, dissolving the crushed ore in a certain amount of water, and carrying out solid-liquid separation to obtain insoluble substances to obtain filtrate;
s2, separating trace impurity ions from the filtrate obtained in the step S1 by adopting a nanofiltration separation technology to obtain a refined sodium chloride solution, and controlling the nanofiltration process condition to be that the membrane area is 0.5m2The nanofiltration pressure is 2.0MPa, and the nanofiltration time is 1.5 h;
s3, adding food-grade potassium chloride with a certain mass into the sodium chloride solution obtained in the S2 to prepare an unsaturated solution at normal temperature, wherein the mass fraction of sodium chloride in the unsaturated solution is controlled to be 18.3-21.6%, and the mass fraction of potassium chloride is controlled to be 5.4-9.8%;
s4, adding lysine nutrient substances accounting for 0.3 percent of the total mass of the sodium chloride and the potassium chloride into the unsaturated solution obtained in the step S3, and carrying out suspension stirring for 1.5h at normal temperature, wherein the stirring speed is 300 r/min;
s5, carrying out ion spray drying on the suspension obtained in the step S4, controlling the solution feeding pump speed to be 300mL/min, the rotation speed of an atomizer to be 12000r/min, the air inlet temperature to be 190 ℃ and the air outlet temperature to be 90 ℃, and preparing micron-sized superfine spherical-structure low sodium salt, wherein the main components of the low sodium salt comprise 73.5% of sodium chloride, 26.4% of potassium chloride and 0.3% of nutrient substance lysine; the particle size distribution of the product is uniform, and the average particle size is 35 mu m; the sphericity was 92%. Compared with common low-sodium salt, the product has the effect of supplementing amino acid.
Example 3
A spray preparation method of low sodium salt with a spherical structure comprises the following specific steps:
s1, crushing natural sylvite ore, dissolving the crushed ore in a certain amount of water, and carrying out solid-liquid separation to obtain insoluble substances to obtain filtrate;
s2, separating trace impurity ions from the filtrate obtained in the step S1 by adopting a nanofiltration separation technology to obtain a refined sodium chloride solution, and controlling the nanofiltration process condition to be that the membrane area is 0.8m2The nanofiltration pressure is 3.0MPa, and the nanofiltration time is 1 h;
s3, adding food-grade potassium chloride with a certain mass into the sodium chloride solution obtained in the S2 to prepare an unsaturated solution at normal temperature, wherein the mass fraction of sodium chloride in the unsaturated solution is controlled to be 18.3-21.6%, and the mass fraction of potassium chloride is controlled to be 5.4-9.8%;
s4, adding calcium gluconate nutrient substances accounting for 0.5 percent of the total mass of the sodium chloride and the potassium chloride into the unsaturated solution obtained in the step S3, and carrying out suspension stirring for 2 hours at normal temperature, wherein the stirring speed is 250 r/min;
s5, carrying out ion spray drying on the suspension obtained in the step S4, controlling the solution feeding pump speed to be 250mL/min, the atomizer rotating speed to be 11000r/min, the air inlet temperature to be 180 ℃ and the air outlet temperature to be 80 ℃, and preparing the micron-sized superfine spherical low-sodium salt. The main components of the low-sodium salt comprise 70.5 percent of sodium chloride, 29.4 percent of potassium chloride and 0.5 percent of nutrient calcium gluconate; the particle size distribution of the product is uniform, and the average particle size is 40 mu m; the sphericity was 93.5%. Compared with common low-sodium salt, the product has the effect of supplementing calcium.
Example 4
A spray preparation method of low sodium salt with a spherical structure comprises the following specific steps:
s1, dissolving common food-grade sodium chloride in a certain amount of water, separating out trace impurity ions from the obtained solution by adopting a nanofiltration separation technology to obtain a refined sodium chloride solution, and controlling the nanofiltration process condition to be membrane area of 1.0m2The nanofiltration pressure is 3.0MPa, and the nanofiltration time is 1 h;
s2, adding food-grade potassium chloride with a certain mass into the sodium chloride solution obtained in the S1 to prepare an unsaturated solution at normal temperature, wherein the mass fraction of sodium chloride in the unsaturated solution is controlled to be 18.3-21.6%, and the mass fraction of potassium chloride is controlled to be 5.4-9.8%;
s3, adding 1.0 percent of vitamin A and vitamin D nutrient substances relative to the total mass of the sodium chloride and the potassium chloride into the unsaturated solution obtained in the step S2, and carrying out suspension stirring for 0.5h at normal temperature, wherein the stirring speed is 500 r/min;
s4, carrying out ion spray drying on the suspension obtained in the step S3, controlling the solution feeding pump speed to be 400mL/min, the atomizer rotating speed to be 15000r/min, the air inlet temperature to be 210 ℃ and the air outlet temperature to be 110 ℃, and preparing micron-sized superfine spherical-structure low sodium salt, wherein the main component of the low sodium salt is 67.5% of sodium chloride, 32.4% of potassium chloride and 1.0% of vitamin A and vitamin D; the particle size distribution of the product is uniform, and the average particle size is 28 mu m; the sphericity is 90%. Compared with common low-sodium salt, the product has the effect of supplementing vitamins.
The content and morphology of the low sodium salt obtained in examples 1-4 were determined according to the QB/T2019-2020 low sodium salt standard, and the results are shown in Table 1; the particle size and morphology of the low sodium salt obtained by the invention were analyzed by a malvern particle size analyzer, a scanning electron microscope and an energy scattering spectrometer, and the results are shown in fig. 1 to 4.
TABLE 1 composition content and morphology of low sodium salt
Figure BDA0003499066740000101
The results in Table 1 show that the low-sodium salt prepared by the method disclosed by the invention can reach the standard of QB/T2019-.
As can be seen from figure 1, the low-sodium nutritive salt product prepared by the method has unimodal particle size distribution, narrow and uniform particle size distribution, small average particle size, no caking phenomenon and good mobile phase; as can be seen from fig. 2-3, the product particles are spherical aggregates, achieving the effect of spherical granulation, and because the direct contact area of the spherical particles is smaller, the negative agglomeration of common cubic salt under the high viscosity of nutrient substances can be effectively avoided, thereby effectively reducing the particle adhesion and agglomeration in the spray drying process and having better anti-caking property; as can be seen from the energy spectrum analysis of FIG. 4, the product particles have compact surfaces, and potassium, sodium and chlorine elements are uniformly distributed and are uniformly embedded in the same spherical particle, thereby indicating that sodium chloride and potassium chloride are uniformly distributed and embedded in the same spherical particle, and micronutrients are uniformly dispersed on the surface or around the spherical particle.
Finally, it should be emphasized that the above-described preferred embodiments of the present invention are merely examples of implementations, rather than limitations, and that many variations and modifications of the invention are possible to those skilled in the art, without departing from the spirit and scope of the invention.

Claims (10)

1. The low sodium salt with the spherical structure is characterized in that the main components of the low sodium salt comprise 65-80 wt% of sodium chloride, 20-35 wt% of potassium chloride and 0.003-1.5 wt% of micronutrients;
the shape of the solid particles of the low sodium salt is spherical aggregate particles, the sodium chloride and the potassium chloride are uniformly embedded in each particle, and the micronutrients are uniformly dispersed on the surface or the periphery of the particles.
2. The low sodium salt having a spherical structure according to claim 1, wherein the average particle diameter of the low sodium salt particles is 10 to 200 μm.
3. The low sodium salt with a globular structure according to claim 1, wherein the sphericity of the low sodium salt is more than 90%.
4. The spray preparation method of low sodium salt with spherical structure according to any one of claims 1 to 3, characterized by comprising the following specific steps:
s1, crushing a main raw material, dissolving the main raw material in a certain amount of water, and carrying out solid-liquid separation to obtain insoluble substances to obtain a filtrate;
s2, separating trace impurity ions from the filtrate obtained in the step S1 by adopting a nanofiltration separation technology to obtain a refined sodium chloride solution with the mass fraction of NaCl lower than 25% and the content of the impurity ions lower than 0.5%;
s3, adding food-grade potassium chloride with a certain mass into the sodium chloride solution obtained in the S2 to prepare an unsaturated solution at normal temperature;
s4, adding nutrient substances into the unsaturated solution obtained in the step S3, and carrying out suspension stirring for 0.5-3h at normal temperature at the stirring speed of 200-600 r/min;
s5, carrying out ion spray drying on the suspension obtained in the step S4 to prepare the micron-sized superfine spherical low-sodium salt.
5. The spray preparation method of low sodium salt with spherical structure according to claim 4, wherein in S1, the main raw material is one or more of natural crystalline stone salt ore, natural argillite salt ore, natural sylvine salt ore and food grade sodium chloride.
6. The method for preparing spray with spherical low-sodium salt according to claim 4, wherein in S4, the nutrient is one or more of ferrous gluconate, ferrous citrate, calcium lactate, calcium gluconate, zinc lactate, zinc gluconate, potassium iodate, sodium selenite, vitamin A, vitamin D, vitamin E, lysine, phenylalanine, tryptophan, and glutamic acid at any ratio.
7. The spray preparation method of low sodium salt with spherical structure according to claim 4, wherein in S2, the process conditions of the nanofiltration separation technology are as follows: the membrane area is 0.24-1.0m2The nanofiltration pressure is 0.5-3.0MPa, and the nanofiltration time is 0.5-3 h.
8. The spray preparation method of low sodium salt with spherical structure according to claim 4, characterized in that in S3, the mass fraction of sodium chloride in the unsaturated solution is controlled to be 18.3-21.6% and the mass fraction of potassium chloride is controlled to be 5.4-9.8% by controlling the addition amount of potassium chloride.
9. The spray preparation method of low sodium salt with spherical structure according to claim 4, wherein the nutrient is added in an amount of 0.005-1.5% by mass of the total mass of sodium chloride and potassium chloride in S4.
10. The spray preparation method of low sodium salt with spherical structure as claimed in claim 4, wherein in S5, the solution feeding pump speed is adjusted to 50-400mL/min, the atomizer rotation speed is 7500-20000r/min, the air inlet temperature is 180-220 ℃, and the air outlet temperature is 80-110 ℃ during the spray centrifugal drying.
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