Compacted products from non-caking salt

FIELD: chemical industry, agriculture, in particular hardness removal agent and saltlick for cattle.

SUBSTANCE: salt with pH 4-10 is pressed under 5000-2500 N/cm2. Salt contains NaCl, less than 0.1 wt.% of water, and iron-ammonium complex of polyhydroxycarboxylic acid in amount sufficient to obtain non-caking salt. As iron-ammonium complex of polyhydroxycarboxylic acid iron-ammonium citrate with molar ratio of iron to citrate-ion from 0.5 to 2 and molar ratio of ammonium to citrate-ion from 0.5 to 2 may be used. Finished product contains 0.1-20 mg/kg of iron and has form of briquettes, balls, bars, crushed plates, tablets, etc. Invention makes it possible to provide good formability under high pressure and conserve pressed product shape in moist medium for a long time.

EFFECT: products from salt non-caking at storage and conveyance.

11 cl, 6 tbl, 2 dwg, 7 ex

 

The present invention relates to a method of manufacturing laminated products of the crystalline non-caking salt, obtained products and their application.

Pressed products of salts are well known. Examples of such products are large pieces of salt (lisanti" for cattle) and small briquettes or tablets salt for use in installations for water softening. Typically, these molded products are made of salt that does not contain protivosvertyvayuschih additives.

However, when using salt not containing protivosvertyvayuschih additives, it will be cake during storage, and therefore will need to take special measures, such as pressing immediately after its production. In practice, this means that the pressing need to spend directly on the company producing salt, which is undesirable. Use normal salt additives, prevent caking, will prevent sliianie salt during storage, but will interfere with the process of pressing of salt in some form. In addition, if you use salt that contains the most frequently used protivozmeinaya supplements - ferrocyanide sodium or potassium, extruded, molded products break easily, especially if they are submerged in the brine. This means that the brine will be more small crystals of salt, that is, "Eliza" (mushing), which can lead to clogged filters, supply pipes and the like, which is undesirable.

The authors of this invention have unexpectedly discovered that the use of a salt containing one or more specific substances, prevent caking, does not lead to caking under normal storage conditions, i.e. in bunkers or in big bags of 1000 kg, which is also referred to as flexible containers average volume (FIBC). However, this does not caking salt can be obtained molded products, such as lumps, pellets and tablets, which will retain its shape, even if you put them in the brine for a period of time at least three weeks, preferably six weeks, and which are characterized by a low level of education "gruel". Still not clear why a substance that prevents caking at low pressures (transport and storage), does not prevent the formation of compacted products under high pressure.

Accordingly, the invention relates to the use of salt containing one or more iron-ammonium complexes, hydroxycarboxylic acids, preferably iron-ammonium citrate complexes as additives, prevent caking, and use the pressed products.

It should be noted that the salt containing iron-ammonium C is tratie complexes as additives, prevent caking, known in the art. Cm. for example, the United Kingdom patent 908017, article Y.Yonei, T.Masuzawa in Nippon Kaisui Gakkai-Shi, 26 143, 1973, pp. 265-272 and articles A. Yamashita et al. in Nippon Sembai Kosha Chuo Kenkyusho Kenkyu Hokoku, 3, 1969, pp.211-247. In the above publication describes that the various iron-ammonium citrate complexes were evaluated for impact on sliianie salt. Tests for evaluation of caking was a common experiments in which simulated pressure acting on salt during storage and transportation. More specifically, tests of sliianie in the work Yonei, Masuzawa included pressing salts containing treated water in the mold under a pressure of 1000 N/cm2and in the work of Yamashita et al. describes the test on sliianie using a pressure of 500 to 1000 N/cm2or test that assessed sliianie heap of salt.

None of the songs "crystalline non-caking" salt not tested, in which salt was molded under a pressure in the range of 5000-25000 N/cm2. The authors found that crystalline non-caking salt composition on the basis of preventing caking of iron-ammonium complex with a hydroxycarboxylic acid, and especially crystalline non-caking salt composition on the basis of iron ammonium citrate complex, show excellent ability to caking/form at these pressur is s, and as a result form a stable compacted products. The expression "stable compacted products" means the products are not destroyed and/or do not form crystals or fragments of size 1 mm3or less when they are immersed in the brine at 20°at 3 weeks, and/or passing the test on the formation of "pulp", as described below.

The pressure used to obtain a stable compacted products, is preferably 5000-20000 N/cm2. The shape of the pressed product has no value, and they may have the form of pellets, rods, beads (including balls with an average diameter of about 2 mm), tablets (broken) plates, stones, or pads, etc. Specialist will easily determine what pressure is best used to manufacture any of these products in various forms, by analyzing the molded products. Observed the successful formation of briquettes under pressure 9000-10000 N/cm2, tablets - under pressure 7000-10000 N/cm2plates under a pressure of about 20,000 N/cm2and balls/pads under pressure 15000-20000 N/cm2; however, the invention should not be limited to these pressures.

The term "salt" in this description is used to denote all the salts that contain more than 25 wt.% NaCl. Preferably, this salt contains more than 50 wt.% NaCl, whereas salt containing more than 99 wt.% NCl, is the most preferred. Preferably, the salt contains less than 5 wt.% water. More preferably, the salt contains less than 3 wt.%, even more preferably less than 1 wt.%, and most preferably less than 0.5 wt.% water. Most suitable for use in the method according to the invention is a salt containing up to 0.1 wt.% water. Salt may be a salt rock, salt, evaporated by the sun, salt, evaporated from the brine, etc.

Exepalikuonis acid that can be used in this invention are selected from compounds having from 3 to 10 carbon atoms, one or more hydroxyl groups and two or more carboxyl groups or mixtures of such acids. Preferably exepalikuonis acid include citric acid, tartaric acid, gluconic acid, sugar acid, mucus acids and their isomers. It was found that iron-ammonium complexes of these oksipiridilovykh acids give salt nasleduemoe at low concentrations. Even more preferred are mixtures oksipiridilovykh acids containing citric acid.

The preferred interval of pH levels for crystalline non-caking salt containing iron-ammonium complex axiolichbiala acid, measured as described below, depends on the specific complexes axiolichbiala acid that Pris is stuut in salt. For example, Yonei reports that for the preferred iron-ammonium citrate complexes preferred range of pH is 7 to 14, preferably about 8.5-9. However, Yama-shita et al. indicate that, depending on the ratio of iron and ammonium complexes will have different pH when dissolved in water, and the pH of the solution containing iron ammonium citrate, which is dispersed in the Sol, which is the preferred method of introduction into granules of salt substances that prevent caking, it is preferable to maintain about 5.5. Which is exactly the range of pH works best for your specific iron-ammonium complex with axiolichbiala acid, can be installed simply by evaluating the caking and the formation of a dispersion of fine particles of salt-treated iron-ammonium complexes of these acids at different pH values. It was found that the preferred range of pH for salesonlinevuh complexes according to the invention is from 4 to 10. More preferably, the pH is from 5 to 7, while the citrate complex was found that the most preferred pH is about 6.

If necessary, the pH can be adjusted using any conventional acid or any reason. Acid or base can be added separately or together with a substance that prevents caking. P is edocfile solution containing one or more iron-ammonium complexes axiolichbiala acid, and the pH regulator is added to salt. The method of introducing substances that prevent caking, and acid or base depends on the desired water content in the resulting salt and water content in salt before processing. In a typical case, the salt spray concentrated solution with additives. Additives can be added either to wet or dry salt. In addition, processed salt can be dried, if desired. Preferably the salt, containing about 2.5 wt.% water, for example, after centrifugation or another stage of the technological process, is treated with a substance that prevents caking, and possibly, a substance that regulates the pH, and then dried. You can also use salt with higher initial water content. Preferably, the treated salt is dried so that the water content was less than 1 wt.%, more preferably less than 0.5 wt.% and most preferably less than 0.1 wt.% by weight of the final product. As a result of such operations are salt, which is loose and which is better suited for molding according to the present invention.

Optionally, you can add salt and/or fluid to handle the additional pH buffer. Use buffers of conventional type. Prefer the LNO they are organic acids. More preferably, they represent a carboxylic acid. Selected acid must be in aqueous solution, the value of RK about the desired pH, as is well known in this field. The buffer can be applied using the (optional) pH regulator and without it. The buffer can be introduced into the composition of salt by spraying pure compounds, a separate solution, and/or after mixing it with a solution for processing against caking. Preferably, the solution for treatment against caking, sprayed on the salt, contains a source of iron, a source of ammonium, exepalikuonis acid, preferably citric acid, possibly, a pH regulator, and possibly pH buffer.

If desired, the solution for treatment containing iron-ammonium complex with axiolichbiala acid, may contain NaCl. Discovered that such containing NaCl solutions were more effective to give a salt of nasleduemoe than solutions based on the normal water. Preferably, such solutions contain 15-25%, more preferably 20-25 wt.% NaCl. It should be noted that other salts such as KCl and/or NH4Cl can also be used to replace (partial) NaCl.

In addition, such solutions for processing salt can optionally contain substances that form complexes with ions of SB, such as hexametaphosphate. The best results b is obtained that when the hexametaphosphate is used with a combination of iron ammonium citrate. In addition, it may be appropriate, depending on the quality of the iron-ammonium complex, first processing complex of hydrogen peroxide (H2About2to increase its effectiveness, as it is known in this field, see, for example, A.A.Yamashita et al., Nippon Sembai Kosha Chuo Kenkusho Kenkyu Hokoku, 3, 1969, pp.231-237.

Since the valency of iron in the salt and the ratio of iron to ammonium may change because along with the ammonium ions may be ions of Na, K, mg, and/or CA, and since this invention may be used various types oksipiridilovykh acids with different number of carboxyl groups, the molar ratio of iron to axiolichbiala acid, and the ratio of ammonium to axiolichbiala acid can vary within wide limits. Successfully used as the ions of divalent and trivalent ions of iron (ferro - and Ferri-ions, respectively). Almost iron in the final composition of the salt may be present in both valence forms. Therefore, the term "iron-ammonium complex axiolichbiala acid", as used throughout this document, it usually refers to a composition containing iron ions of different valency, ammonium ions and at least one group exopoli arbonboy acid in ionic form.

The number axiolichbiala acid relative to the amount of iron ions may depend on whether ferro - or Ferri-ions, the ratio of iron ions to ammonium ions, from the presence of the complex, for example, ions of Na, K, mg, and/or CA and from nature axiolichbiala acid, particularly on the number of carboxyl groups per mole of acid. Preferably, the iron-ammonium complex is neutral in charge. For iron-ammonium citrate, which is preferred, prevent caking, a suitable molar ratio of iron to citrate ions is the ratio of from 0.5 to 2. The molar ratio of ammonium ions to citrate ions may vary within wide limits depending on, inter alia, from ions that are part of the complex. The preferred molar ratio of ammonium ions to citrate ions ranges from 0.5 to 2. For the preferred iron-ammonium citrate was found that is suitable molar ratio of citric acid to ammonium ion and iron ion is about 1:1:1. This ratio was also found in commercial grades of iron ammonium citrate, used in the examples.

Iron-ammonium complexes axiolichbiala acid is preferably used in an amount such that the end does not caking salt composition was 0,1-0 mg of iron per kg of composition. It is preferable to introduce 0.25 to 10 mg of iron per kg of the composition, and most preferably the number entered iron is 0.5-7 mg/kg To reduce the formation of a dispersion of fine particles of the pressed product number used iron-ammonium complex axiolichbiala acid preferably chosen closer to the bottom border of the specified interval. For granules of salt in the form of pebbles, containing citrate ferric ammonium characterized by a low degree of formation of a dispersion of fine particles, the preferred amount of iron is in the range from 0.5 to 3.5 mg per kg of product, and most preferably in the range of 0,5-2,5 mg/kg

If required, the present invention can also be used conventional additives, prevent caking, together with the agent against caking according to the invention, provided that the introduction of such conventional additives will not have any adverse effect on sliianie salt and/or on the properties of pressed products, especially on tensile fracture and the tendency to form a "slurry". If you use this combination protivosvertyvayuschih substances, it is preferable to use less than 50 wt.%, more preferably less than 25 wt.%, even more preferably less than 10 wt.% and most preferably less than 5 wt.% conventional additives that prevent slieve the Oia, from the total mass of all used protivosvertyvayuschih additives.

Molded products obtained by the method according to the invention, suitable for use as pieces of salt, but preferably are used in cases that require a high wet tensile fracture. Wet tensile fracture is usually required in those operations where the salt is dissolved periodic or continuous manner, when the salt is usually submerged in the brine. Examples of such operations usually can be found in installations where the regeneration of ion exchange resins with the use of brine, as is known in the art. In accordance with this molded products according to the invention is best suited for use in devices for dissolving salt for water softening.

EXPERIMENTAL PART

the pH of the salt was changed as follows:

First, at a temperature of 20°prepare a saturated solution of NaCl (brine), in which the pH is brought to 7 using NaOH and/or Hcl. Then 100 g of the analyzed salt was added to 100 ml of brine, and the resulting suspension was stirred 10 minutes at 20°C. the pH Value of the suspension after the specified mixing was measured to estimate the pH of salt.

Water adsorbed salt was determined by measuring the weight loss at drying, exposing 27.5 g of salt to the action of microwave radiation power IU the greater least 600 watts for 20 minutes.

Caking or free-flowing salt was determined using a rectangular chamber, as shown in figa. After keeping the salt in this chamber for a certain period of time, putting salt transversely climate impact and effect of a certain load, which corresponds to the normal conditions of storage and processing of salt (see examples), opened the valve at a rate of 0.2 mm/s, leading to the situation depicted in fig.1b. The flowability was evaluated on the basis of gap width required to salt flowed through this slit, and the average angle of repose of the remaining material.

"Wet" and "dry" tensile fracture was determined by measuring the force required to fracture a compressed tablet, placed in the torque sensor. Tablets were made on a laboratory press Herrog HTP 40 (1993) with an adjustable pressing force. The force exerted on the salt, was 7850 N/cm2. The tablet diameter was equal to 2.5 cm, and weight - 15 year

The dry strength was measured after put the pressed product in the ambient air. Wet strength was measured after the pressed product was immersed in a saturated solution of NaCl for a certain period of time.

In both examples, the tensile fracture was defined as the maximum force, the impact of which can be that is tapped, lying on its side, before its destruction, divided by the surface area destruction. Tablet usually breaks in the middle. Therefore, ultimate tensile stress (strength) is calculated from the measured maximum effort and sizes of tablets, according to the following formula. Formula:

in which

σ=ultimate tensile stress (N/cm2)

Fmax=maximum breaking force (kg)

D=the diameter of the tablets (cm)

w=thickness of the tablets (cm)

The formation of a dispersion of fine particles of the pressed products of salts was evaluated on the basis of instructions Pellet Mush Volume Test", published by the firm "Culter - Magner Salt Company. A it is about 860 g undamaged pressed products ("pebbles", pills, etc.) was collected and transferred into a cylinder with a diameter of 12.5 cm and a height of 18 see Then added 1 l of distilled water and the cylinder was closed. The cylinder was placed in a device for mixing by shaking the turbula T2F and was shaken for 20 minutes at room temperature at a speed of about 45 rpm the Resulting saturated brine decantation and preserved for subsequent leaching. The remaining mixture of salt and brine was poured into the sieve with the hole diameter of 2.36 mm (8 mesh) and washed with brine. The filtrate, containing very small particles, collected and cone "Imhoff" to defend. After settling into the tech is of 30 minutes at the bottom of the cone was determined by the number of "pulp", that is, the amount of particles in the specified brine collected at the bottom of the cone. To successfully pass this test, salt should form less than 20 ml of the slurry. Preferably, the resultant dispersion of fine particles should be below 15 ml, more preferably below 10 ml and most preferably below 5 ml.

In experiment 1 used an iron ammonium citrate firm "Fluka" called "ammonium Citrate iron, brown No. 09714. Analysis of this product showed that it contained approximately 64 g/kg NH4, 205 g/kg Fe and 585 g/kg citrate. In subsequent experiments used the iron-ammonium citrate firm "Paul Lohman", which contained about 78 g/kg NH4, 200 g/kg Fe and 615 g/kg citrate.

EXAMPLE 1 AND COMPARATIVE EXAMPLES a and b

Salt with a water content of less than 0.1 weight. % and pH 8.5) was mixed with a solution containing 17 g/l protivosvertyvayuschih agent specified in table 45 g/l H2SO4and 250 g/l NaCl. Only used with 0.55 ml of solution per 1 kg of salt. The resulting mixture was dried at 60°using the dryer with a movable layer, so that the water content in the resulting composition of the salt was less than 0.1 wt.%. The pH of the salt obtained was in the range of 6 to 6.5. After tabletting defined "dry" destructive force immediately upon receipt, i.e. within 1 hour after pressing the last tablet, and after 24 cha is A.

Table
ExampleSalt composition0 hours24 hours
 protfolio living agent -mg/kgH/cm2H/cm2
Andno-119195
InFerrocyanide of potassium4 (based on Fe(CN)63423
1iron ammonium citrate2 (based on Fe)9288

"Dry" strength salt containing iron-ammonium citrate complex was higher than the strength of the pressed products derived from salts containing normal protivosvertyvayuschih agent. Wet strength of the same pressed products were determined through a different number of days, as shown in the following table. Wet strength (stress fracture) is expressed in H/cm2.

Table
ExampleThe days of immersion in brine
 0146 814212842
And1199110910210670795764
In3400000000
19210014612313160809365

It is obvious that for tablets of salt containing iron-ammonium citrate complex, requires a destructive force, which is much higher than that of products, pressed salt with traditional protivosnaryadnym agent and at least the same as wet destructive force for salt, which does not contain protivosvertyvayuschih agent.

The flowability of salt, which was used for the manufacture of laminated products in the above examples was determined by measuring the flowability of salt using the device described above. In one example, saturated salt water, to increase its content of moisture. Before testing salt was first kondicionirovanie in the specified device using the next daily cycle: 2 hours at 10°C/90% RH the Sith. humidity, 2 hours at 25°C/50% relates. humidity (RH), 2 hours at 10°C/90% RH and 18 hours at 15°C/70% RH.

Table
Example3 day air-conditioning, a pressure of 0.1 N/cm2humidity less than 0.1 weight. %2 day air-conditioning, pressure 5 H/cm2the moisture content of 0.1 weight. %3 day air pressure of 5 N/cm2the moisture content of 2.5 weight. %
Ando/+about-
In+o/+o/+
1o/++o/+
- = marked, sliianie, o = some pieces + = free for

Table
ExampleThe minimum required slit width (mm)
 3 days. air pressure of 0.1 N/cm2, humidity less than 0.1 weight. %2 DN. air pressure of 5 N/cm2the moisture content of 0.1 weight. %3 days. air pressure 5 H/cm2the moisture content of 2.5 weight. %
And63more than 150
In32more than 150
132more than 150

Table
ExampleThe average angle of the slope of the residual material
 3 days. Air pressure of 0.1 N/cm2, humidity less than 0.1 weight. %2 DN. air pressure 5 H/cm2the moisture content of 0.1 weight. %3 days. air pressure of 5 N/cm2the moisture content of 2.5 weight. %
And5540the concentration is
In3637the concentration is
13637the concentration is
N.O.=not determined

The results imply that the flowability is not pressed salt containing iron ammonium citrate, is as good as the flowability of salt, containing the usual protivozmeinaya agents and much better flowability of salt, which does not contain protivosvertyvayuschih agents. However, at the same time, the pressed product according to the invention is as durable as molded products obtained from the salt that does not contain protivosvertyvayuschih is hentov, but it is much stronger than salt containing traditional protivosvertyvayuschih agent.

EXAMPLES 2-4 AND COMPARATIVE EXAMPLE

In these examples investigated the influence of the number of added protivosvertyvayuschih agent on the strength of the extruded product. The pH value of the salt is not regulated. Accordingly, a salt with a water content less than 0.1 wt.% was mixed with a solution containing 17 g/l of iron ammonium citrate, if it was used that corresponded to the iron content of about 3.4 g/l and NaCl 250 g/l In experiments 2-4 were used to 0.29, of 0.58 and 0.88 ml of the indicated solution per kg of salt, respectively, in order to add those amounts, prevent caking, which are listed in the table below. The resulting mixture was dried at 60°in the dryer fluidized bed so that the water content in the resulting composition of the salt was less than 0.1 wt.%. Then extruded tablets, as described above. It should be noted that the number of iron tablets was slightly higher than the number added with a substance that prevents caking due to the presence of some amounts of iron in the treated salt. Analysis of the tablets showed that the total iron content is in the range from 0.9 mg/kg in the comparative example to 4.4 mg/kg in example 4.

Dry strength (breaking force dry when standing) were determined in tablets immediately after their receipt, i.e. within 1 hour after pressing the last tablet, and after 24 hours. Wet strength was determined after 1 and 3 weeks of curing in brine. The results are presented in the following table.

Table
ExampleQty protivosvertyvayuschih agentDry strengthWet strength
  0 hours24 hours7 days21 days
 mg/kgN/cm2N/cm2N/cm2N/cm2
no10925111297
21782208385
3281175105114
43661589198

From the table it is clear that the amount of iron ammonium citrate, which corresponds to 2-3 mg/kg of iron, gives a very good strength, both dry and wet. Processed salt in examples 2-4 pok which shows acceptable properties, characterizing reduced caking, at pH values in the range of 4-10.

EXAMPLES 5-7

The procedure of examples 2-4 were used in the industrial scale to obtain a salt containing iron ammonium citrate in the amount of 1.5, 2 and 3 mg/kg (expressed in mg of iron per 1 kg of tablets), respectively. Sol had acceptable characteristics caking, and from her received "small stones". When tested salt stones on the formation of a slurry was formed volumes of small particles, equal to 1.5, 2 and 1 ml, respectively.

1. A method of manufacturing molded products of the salt by sprasowania salt containing salesonlinevyv complex axiolichbiala acid in a quantity sufficient to give the salt nasleduemoe, and water in an amount less than 1 wt.%, at pressures from 5000 to 25000 N/cm2and salt has a pH from 4 to 10.

2. The method according to claim 1, in which the pressed salt contains less than 0.1 wt.% water.

3. The method according to claim 1 or 2, in which salesonlinevyv complex axiolichbiala acid is used in such amount to enter in the final product is from 0.1 to 20 mg/kg of iron.

4. The method according to any preceding paragraph, in which salesonlinevyv complex axiolichbiala acid is salesonlinevyv citrate.

5. The method according to claim 4, in which the molar ratio of iron to citrate ions is from 05 to 2, and the molar ratio of ammonium to citrate ions is independently from 0.5 to 2.

6. The method according to any preceding paragraph, in which the Sol further comprises a pH buffer.

7. Molded salt products obtained by the method according to any one of claims 1 to 6.

8. Molded salt products according to claim 7, having the form of pellets, rods, beads, tablets, (broken) plates or stones/pads.

9. Salt-lick, characterized in that it is obtained from the molded salt products according to claim 7 or 8.

10. Installation for regeneration of ion exchange resins comprising a device for dissolving salts, characterized in that the quality of the salt it contains molded salt products according to claim 7 or 8.

11. Installation for regeneration of ion exchange resins according to claim 10, characterized in that it is part of the installation for water softening.

Priority points and features:

18.05.2000 according to claim 5 in part a characteristic “molar ratio of ammonium to citrate ions... from 0.5 to 2.



 

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6 cl, 5 tbl, 4 ex

FIELD: mineral fertilizers.

SUBSTANCE: invention relates to ammonium nitrate-based fertilizer manufacture and consists in treatment of ammonium nitrate granules with solution containing chemical reagent and inert component, the former being potassium sulfate aqueous solution, with which prilled ammonium nitrate granules are treated at 40-50°C followed by treating granules with phosphogypsum (inert component) having moisture content 2-3% and grinding fineness no larger than 30 μm until its percentage in the granules attains 1-20%.

EFFECT: preserved high strength of ammonium nitrate granules at greater number of thermal cycles at temperatures 20 to 50C and increased temperature resistance.

3 cl, 1 tbl, 6 ex

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