CN115868619B - Composite anticaking agent for edible mineral salt and preparation method thereof - Google Patents

Composite anticaking agent for edible mineral salt and preparation method thereof Download PDF

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Publication number
CN115868619B
CN115868619B CN202211625017.7A CN202211625017A CN115868619B CN 115868619 B CN115868619 B CN 115868619B CN 202211625017 A CN202211625017 A CN 202211625017A CN 115868619 B CN115868619 B CN 115868619B
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salt
calcium silicate
particle size
ultrasonic
ammonium citrate
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CN115868619A (en
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黄承
仇耀军
程文波
蒋海斌
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Jiangsu Salt Industry Research Institute Co ltd
Jiangsu Suyan Jingshen Co ltd
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Jiangsu Salt Industry Research Institute Co ltd
Jiangsu Suyan Jingshen Co ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A40/00Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
    • Y02A40/90Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in food processing or handling, e.g. food conservation

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Abstract

The invention relates to a compound anti-caking agent for salt, which comprises or consists of acacia, calcium silicate and ferric ammonium citrate; the composite anticaking agent comprises the following components in percentage by mass of the salt: 0.04% -0.2% of acacia; 0.1 to 0.4 percent of calcium silicate; ferric ammonium citrate 0.0008-0.0025%. The composite anticaking agent for salt has excellent anticaking effect, does not contain cyanide, and is safer and more reliable to eat.

Description

Composite anticaking agent for edible mineral salt and preparation method thereof
Technical Field
The invention belongs to the field of food additives, and particularly relates to a composite anti-caking agent for edible mineral salt and a preparation method thereof.
Technical Field
The inherent caking property of salt, i.e. the original loose state is mutually stuck into a block, which is inconvenient to transport, store and use, restricts the performance of the salt, and the addition of anti-caking agent in salt is studied for preventing the caking of the salt in various countries of the world.
At present, potassium ferrocyanide is mostly adopted as an anticaking agent in refined edible salt, food processing salt and industrial refined salt in China. The anti-caking mechanism is to change the grain size distribution of the salt when the salt is recrystallized under the influence of external environment, so that the crystal grains of the salt do not form cross-linking, thereby preventing the salt from caking in the storage process, and the salt has the characteristics of small addition amount and good caking effect. However, the molecular structure of the salt contains cyanide groups, so that people are liable to worry about the quality safety of the salt. The potassium ferrocyanide added in the salt of the national standard GB 2760 national Standard for food safety food additive use Standard (food safety national Standard) is 0-0.025mg/kg, which can not cause harm to human body.
With the progress of society and the improvement of the living standard of people, people put higher demands on physical health and food safety, and NY/T1040-2006 standard of green food edible salt, wherein the standard clearly prescribes that the green food edible salt does not allow the addition of potassium ferrocyanide, but allows the addition of anti-caking agents such as ferric ammonium citrate, silicon dioxide, calcium silicate, ferric tartrate and the like. When the silicon dioxide and the calcium silicate are used for the salt anti-caking agent, the anti-caking effect can be achieved only by generally larger dosage, and indexes of sodium chloride and water insoluble substances in the salt are easy to be unqualified; the amount of the ferric tartrate is very small, the anti-caking effect is good, but the price is high, and the method for detecting the ferric tartrate in the salt is not available, so the method cannot be applied to the salt; the ferric ammonium citrate has color, and the whiteness of the salt is reduced when the ferric ammonium citrate is added into the salt.
Chinese patent CN107019200a discloses a compound edible salt anticaking agent and its preparation method, the anticaking agent mainly comprises silicon dioxide, magnesium carbonate and tricalcium phosphate; chinese patent CN101658254a discloses a compound anticaking agent for table salt, which mainly consists of ferric ammonium citrate, tricalcium phosphate, and calcium stearate. However, according to GB 2760 issued by the Ministry of health of China and the annual announcements, magnesium carbonate, tricalcium phosphate and calcium stearate cannot be used as anti-caking agents for salt.
In summary, the market demands for salt products without potassium ferrocyanide anticaking agents are urgent, and the development of novel salt anticaking agents which are capable of replacing potassium ferrocyanide, meet the national legal and legal requirements and are economical and reasonable has become urgent matters for salt manufacturing enterprises.
Disclosure of Invention
The invention aims to provide a composite anti-caking agent for salt, which does not contain cyanide, is nontoxic and harmless and has good anti-caking effect, and a preparation method thereof, and aims to solve the problem that the traditional salt anti-caking agent (potassium ferrocyanide) brings about concern to consumers about salt safety.
In order to achieve the above object, the present invention provides a composite anti-caking agent for salt: the compound anticaking agent comprises or consists of acacia, calcium silicate and ferric ammonium citrate; the anti-caking agent comprises the following components in percentage by mass:
gum arabic 0.04% -0.2%, preferably 0.05% -0.1%, still preferably 0.06% -0.09%; 0.1 to 0.4%, preferably 0.15 to 0.35%, and still preferably 0.2 to 0.3% of calcium silicate; ferric ammonium citrate 0.0008-0.0025%, preferably 0.001-0.002%, and still preferably 0.001-0.0015%.
The acacia, calcium silicate and ferric ammonium citrate are all food-grade.
The particle size range of the anti-caking agent is as follows: the calcium silicate has a specific surface area of 300-600m and a particle size of 1-10 μm, preferably 4-6 μm 2 /g; the ferric ammonium citrate has a particle size of 10 μm or less, preferably 6 μm or less, preferably about 5 μm.
The calcium silicate is preferably calcium silicate with the particle size of less than 6 mu m, which is prepared into slurry by grinding, ultrasonic treatment is carried out on the slurry, and then the slurry is dried, crushed and sieved.
The preparation method of the composite anti-caking agent for salt provided by the invention comprises the following steps:
(1) Pulverizing calcium silicate into powder of 10 μm or less, preferably 6 μm or less; preferably, the calcium silicate is crushed, further ground into slurry, the slurry is subjected to ultrasonic treatment, and then the calcium silicate with the particle size of less than 6 mu m is obtained through drying, crushing and sieving;
(2) Dissolving acacia in water to form an aqueous solution, e.g., at a concentration of 2-20wt%, further e.g., 5-10wt%;
(3) Adding the Arabic gum aqueous solution and ferric ammonium citrate into the salt, mixing, adding the calcium silicate obtained in the step (1), and uniformly mixing again to prepare the composite anticaking agent.
In a specific embodiment, the preparing step comprises:
(1) Grinding calcium silicate according to the particle size requirement, and sieving with a sample separating sieve of 0.15mm to obtain undersize with the particle size smaller than 150 μm;
(2) Placing the undersize material in a ball mill, and ball milling by taking ethanol as a medium to prepare slurry;
(3) Placing the slurry in a container such as a conical flask, placing in an ultrasonic cleaner, and ultrasonically oscillating for 15-120min (preferably 60 min) at a water bath temperature of 30-60deg.C (preferably 40 ℃) under ultrasonic power of 100-200r/min (preferably 150 r/min);
(4) Carrying out suction filtration (for example, vacuum degree is 0.02-0.1 MPa), drying (for example, 70-80 ℃), crushing and grinding the dried material, and then passing through a sample separating sieve with 6 mu m to obtain calcium silicate with particle diameter smaller than 6 mu m after ultrasonic modification;
(5) Adding acacia to water to prepare 5% -10% acacia solution, and adding acacia aqueous solution into salt according to the mass percentage of 0.05% -0.1%; adding ferric ammonium citrate into salt according to the mass percent of 0.001-0.0015%, and uniformly mixing; and (3) adding the calcium silicate obtained in the step (4) according to 0.2-0.3% of the mass percentage of the salt, and uniformly stirring and mixing to prepare the salt product added with the composite anticaking agent.
Compared with other gums such as tragacanth, the low viscosity of the acacia is utilized to enable the ferric ammonium citrate and the calcium cobaltate to be more uniformly distributed and adhered on the surfaces of the salt particles, the moisture absorption and agglomeration tendency of the salt particles is improved by competing moisture absorption with the salt particles, static charges and molecular acting forces on the surfaces of the salt particles are eliminated, the cohesive force between the salt particles is effectively blocked, and the synergistic anti-caking performance of the ferric ammonium citrate and the calcium silicate is enhanced. The combination of the three has outstanding anti-caking effect.
Advantageous effects
Compared with the prior art, the invention has the following advantages and effects:
(1) The composite caking agent provided by the invention is white, and the whiteness of salt is not changed.
(2) The composite anticaking agent of the invention does not contain cyanide, is nontoxic and harmless, and eliminates the mental panic caused by the salt safety problem generated by the traditional salt anticaking agent potassium ferrocyanide.
(3) Through ball milling and ultrasonic vibration, the specific surface area of the calcium silicate is increased, the adsorption capacity of the calcium silicate is enhanced, ferric ammonium citrate and calcium silicate are enabled to be completely adhered and covered on the surface of sodium chloride under the action of low viscosity of Arabic gum, the physical barrier effect is achieved, and the calcium silicate competes with sodium chloride particles for absorbing moisture, so that the moisture absorption and agglomeration tendency of the sodium chloride is improved; meanwhile, static charges and molecular acting forces on the surface of sodium chloride are eliminated, so that the fluidity of salt is improved, and the caking resistance is improved.
(4) The composite anticaking agent can mask the defects and defects of a single anticaking agent, the anticaking effect is obviously better than that of single calcium silicate and ferric ammonium citrate, and the anticaking effect is more obvious.
Detailed Description
In order to facilitate understanding of the present invention, the following description of further information is provided in connection with examples, but embodiments of the present invention are not limited thereto.
Example 1
A compound anticaking agent for well mineral salt and a salt product thereof comprise the following steps:
(1) Weighing 100g of calcium silicate, grinding, sieving with a 0.15mm (100 mesh) sieve, and collecting undersize;
(2) Weighing 20g of undersize material, placing the undersize material into a ball mill, and ball-milling the undersize material by taking 95% ethanol as a medium to prepare slurry;
(3) Placing the obtained slurry in an conical flask, placing in an ultrasonic cleaner, and performing ultrasonic oscillation for 60min at the water bath temperature of 40 ℃ under the ultrasonic power of 150 r/min;
(4) Carrying out suction filtration on the ultrasonic slurry under the condition of vacuum degree of 0.05MPa, and drying the obtained filter residues at 80 ℃ after the suction filtration is finished; crushing and grinding the dried material, and sieving to obtain calcium silicate with the particle size smaller than 6 mu m;
(5) Firstly, weighing 10g of acacia gum, dissolving in water to prepare 10% acacia gum aqueous solution by mass percent, and adding the acacia gum aqueous solution into salt according to the mass percent of salt to be 0.05%; secondly, adding ferric ammonium citrate into the salt according to 0.001% of the mass percentage of the salt, and uniformly mixing; and (3) adding the calcium silicate obtained in the step (4) according to 0.3% of the mass percentage of the salt, and stirring and mixing uniformly to prepare the salt product added with the composite anticaking agent (calcium silicate and ferric ammonium citrate).
Example 2
A compound anticaking agent for well mineral salt and a salt product thereof comprise the following steps:
(1) Weighing 200g of calcium silicate, grinding, sieving with a 0.15mm (100 mesh) sieve, and collecting undersize;
(2) Weighing 50g of undersize material, placing the undersize material into a ball mill, and ball-milling the undersize material by taking 95% ethanol as a medium to prepare slurry;
(3) Placing the obtained slurry in an conical flask, placing in an ultrasonic cleaner, and performing ultrasonic oscillation for 50min at the temperature of water bath of 50 ℃ under the ultrasonic power of 120 r/min;
(4) Carrying out suction filtration on the ultrasonic slurry under the condition of vacuum degree of 0.08MPa, and drying the obtained filter residues at 70 ℃ after the suction filtration is finished; crushing and grinding the dried material, and sieving to obtain calcium silicate with the particle size smaller than 6 mu m;
(5) Firstly, weighing 10g of acacia gum, dissolving in water to prepare 10% of acacia gum aqueous solution by mass, and adding the acacia gum aqueous solution into salt according to the mass percentage of 0.1%; and (3) adding ferric ammonium citrate into the salt according to 0.0015% of the mass percentage of the salt, uniformly mixing, adding the calcium silicate obtained in the step (4) according to 0.2% of the mass percentage of the salt, and uniformly stirring and mixing to prepare the salt product added with the composite anticaking agent (calcium silicate and ferric ammonium citrate).
Example 3
A compound anticaking agent for well mineral salt and a salt product thereof comprise the following steps:
(1) Weighing 100g of calcium silicate, grinding, sieving with a 0.15mm (100 mesh) sieve, and collecting undersize;
(2) Weighing 20g of undersize material, placing the undersize material into a ball mill, and ball-milling the undersize material by taking 95% ethanol as a medium to prepare slurry;
(3) Placing the obtained slurry in an conical flask, placing in an ultrasonic cleaner, and performing ultrasonic oscillation for 60min at the water bath temperature of 40 ℃ under the ultrasonic power of 150 r/min;
(4) Carrying out suction filtration on the ultrasonic slurry under the condition of vacuum degree of 0.05MPa, and drying the obtained filter residues at 80 ℃ after the suction filtration is finished; crushing and grinding the dried material, and sieving to obtain calcium silicate with the particle size smaller than 6 mu m;
(5) Firstly, weighing 10g of acacia gum, dissolving in water to prepare 10% of acacia gum aqueous solution by mass, and adding the acacia gum aqueous solution into salt according to the mass percentage of 0.15%; secondly, adding ferric ammonium citrate into the salt according to 0.002 percent of the mass percent of the salt, and uniformly mixing; and (3) adding the calcium silicate obtained in the step (4) according to 0.25% of the mass percentage of the salt, and stirring and mixing uniformly to prepare the salt product added with the composite anticaking agent (calcium silicate and ferric ammonium citrate).
Example 4
Test of anti-caking effect of composite anti-caking agent for well and mineral salt:
1. test object: salt added with potassium ferrocyanide (added amount of potassium ferrocyanide: 10 mg/kg), edible salt added with ferric ammonium citrate (added amount of ferric ammonium citrate: 25 mg/kg), edible salt added with calcium silicate (added amount of calcium silicate: 0.5%), salt added with calcium silicate and ferric ammonium citrate (added amount of calcium silicate: 0.3%, added amount of ferric ammonium citrate: 20 mg/kg), edible salt of the composite anticaking agent of example 1, edible salt without anticaking agent.
2. The test process comprises the following steps:
1. test environment: the temperature is 20+/-5 ℃ and the relative humidity is 60+/-15 percent.
2. Product bagging: the 6 kinds of salt to be tested are respectively filled into plastic sealing bags according to the specification of 350g, and the plastic sealing bags are sealed and stored after being exhausted.
3. Stacking and pressing products: 6 points are equally divided on a flat rectangular platform, 5 samples of each salt are respectively placed at each point, and then a steel plate with the bottom of about 50kg is pressed on.
3. Test results: according to the requirement, 6 products are sampled and observed for anti-caking performance at regular intervals, and the anti-caking effect of the obtained products is shown in table 1.
Compared with other anticaking agents, the composite anticaking agent disclosed by the invention has the advantages that three substances which are uniquely selected have synergistic effect, the specific surface area of the calcium silicate is improved and the adsorption performance of the calcium silicate is enhanced due to the treatment, such as crushing and ultrasonic treatment, meanwhile, the distribution uniformity and the adsorption of the two anticaking agents, namely the calcium silicate and the ferric ammonium citrate, on the surface of salt particles are improved through Arabic gum, the synergistic anticaking effect of the two anticaking agents is enhanced, the anticaking effect is slightly inferior to the anticaking performance of the potassium ferrocyanide, but the anticaking effect is superior to that of other anticaking agents, cyanide is not contained, and the composite anticaking agent is safer and more reliable to eat.

Claims (5)

1. The composite anticaking agent for the salt is characterized in that the acacia gum is 0.05-0.1% by mass of the salt; 0.15 to 0.35 percent of calcium silicate; ferric ammonium citrate of 0.001-0.002%,
wherein, the grain diameter range of the anti-caking agent is as follows: calcium silicate with a specific surface area of 300-600m and a particle size of less than 6 μm 2 /g; the particle size of the ferric ammonium citrate is below 10 mu m,
wherein the calcium silicate is obtained by the steps of:
(1) Grinding calcium silicate according to the particle size requirement, and sieving with a sample separating sieve of 0.15mm to obtain undersize with the particle size smaller than 150 μm;
(2) Placing the undersize material in a ball mill, and ball milling by taking ethanol as a medium to prepare slurry;
(3) Placing the slurry in a container, placing in an ultrasonic cleaner, and applying ultrasonic power of 100-200r/min and ultrasonic power of 30-60 o C, carrying out ultrasonic oscillation for 15-120min at the water bath temperature;
(4) And (3) carrying out suction filtration and drying on the slurry subjected to ultrasonic treatment, crushing and grinding the dried material, and then passing through a sample separating sieve with the diameter of 6 mu m to obtain the calcium silicate with the particle diameter of less than 6 mu m after ultrasonic modification.
2. The composite anticaking agent for salt according to claim 1, wherein the mass percent of the salt is 0.06% -0.09% of acacia; 0.2 to 0.3 percent of calcium silicate; the ferric ammonium citrate is 0.001-0.0015%.
3. The composite anti-caking agent for table salt according to claim 1, wherein the anti-caking agent has a particle size ranging from: calcium silicate 4-6 μm; the particle size of the ferric ammonium citrate is less than 6 mu m.
4. The composite anticaking agent for common salt according to claim 3, wherein the particle size of the ferric ammonium citrate is 5 μm.
5. The preparation method of the salt product added with the composite anticaking agent is characterized by comprising the following steps:
(1) Grinding calcium silicate according to the particle size requirement, and sieving with a sample separating sieve of 0.15mm to obtain undersize with the particle size smaller than 150 μm;
(2) Placing the undersize material in a ball mill, and ball milling by taking ethanol as a medium to prepare slurry;
(3) Placing the slurry in a container, placing in an ultrasonic cleaner, and applying ultrasonic power of 100-200r/min and ultrasonic power of 30-60 o C, carrying out ultrasonic oscillation for 15-120min at the water bath temperature;
(4) Carrying out suction filtration and drying on the slurry subjected to ultrasonic treatment, crushing and grinding the dried material, and then passing through a sample separating sieve with the diameter of 6 mu m to obtain calcium silicate with the particle diameter of less than 6 mu m after ultrasonic modification;
(5) Adding acacia to water to prepare 5% -10% acacia solution, and adding acacia aqueous solution into salt according to the mass percentage of acacia relative to salt of 0.05% -0.1%; adding ferric ammonium citrate into salt according to the mass percent of 0.001-0.002%, and uniformly mixing; and (3) adding the calcium silicate obtained in the step (4) according to 0.15-0.35% of the mass percentage of the salt, and uniformly stirring and mixing to prepare the salt product added with the composite anticaking agent.
CN202211625017.7A 2022-12-16 2022-12-16 Composite anticaking agent for edible mineral salt and preparation method thereof Active CN115868619B (en)

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