Method for preparing concentrated iron chelate solution and iron chelate

FIELD: inorganic chemistry, chemical technology.

SUBSTANCE: invention relates to the improved method for preparing metal complex compounds, in particular, to iron complex (chelate) as its concentrated solution. Method is carried out by interaction of iron salt in an aqueous medium with a chelate-forming agent wherein N,N,N',N'-ethylenediaminetetraacetic acid is used as a chelating agent and citric acid that are added simultaneously or successively. The process is carried out at temperature 70-90°C and in the process of mixing iron salt or after mixing with chelate-forming agent an aqueous solution of ammonia or ammonium citrate is added for providing pH value of the end product 2.0-2.3. The complex-forming agent can comprise succinic acid additionally. Method provides preparing iron chelate as a concentrated solution with the content of iron 60-100 g/l. Invention can be used in agriculture for root and leaf feeding of plants.

EFFECT: improved preparing method.

4 cl, 6 ex

 

The invention relates to the production of complex compounds of metals with chelating agents (of complexions metals), and specifically to complexant (chelate) iron in the form of a concentrated solution, widely used in agriculture for root and foliar nutrition (feeding) plants, as a provider of trace elements in the life of plants and animals.

Thus the invention in particular relates to the production of a solution of trace elements of iron that is intended, in particular, for the root and foliar nutrition (feeding) plants, as well as to compensate for the lack of iron in plant life and animals, man in case of its appearance. The iron chelate is made by yourself or in mixture with macro fertilizers in the case of its application in agriculture.

The need, for example, plants in the gland several times higher than in the other trace elements, therefore, a need for additional feeding (feed) iron supplementation and, respectively, to prepare a separate product containing only iron.

Known methods for producing iron preparations by dissolving its inorganic salts, particularly sulphates in the water, including the introduction of hot water with concentrated sulfuric acid followed by the addition of sulphate of iron.

Weeks the STATCOM method is the relatively low solubility of ferric sulfate even in such conditions, which leads to a low content of trace elements of iron in the finished solution (low concentration), and the iron is still in the inorganic form. This means that the trace is not fully absorbed by the plants, i.e. has low quality, but on the other hand, this solution is not miscible with the solution of macronutrients for simultaneous power plants, since the formation of poorly soluble compounds (inorganic phosphate of iron), which precipitate and impede fertilization (Recommendations for application of fertilizers to obtain the planned yields of high quality vegetable crops on artificial substrates in greenhouses. M., 1991, "Soussaline, TIN, S.11, 12).

Practically there is no way analogous to obtain chelated iron in the form of dissolved concentrate. In commercially available method of obtaining chelate iron in the form of a solution of Fe-EDTA (Fe salt and ethylenediaminetetraacetic acid) content of Fe is only 2-3% (or 20-30 g/l), which reduces the profitability of its transportation't even very long distances due to the large water content (Overview "Application of chelating agents in agriculture". M., 1984, niitekhim, pp.2-3, 6-12).

From SU 1611901 A1, 07.12.1990 a method of obtaining of complexions (chelates) Fe, Mn, Zn and Mo, used for the stern of tea plant. Get chelates interaction carbonates of the respective metals or carbonate ores with oxidation products of molasses or with oxidized hydrolysate syrup plant materials. The resulting chelates metals (in the form of mixtures of chelates metals) is mixed with clinoptilolite tuff and use of such composition. However, well-known invention of the iron chelates get mixed with other metals chelates in the form of a granular mass.

From RU 2059647, 10.05.1996 known method of obtaining complexant iron complex of ascorbic acid with ferric chloride interaction of ascorbic acid with sodium carbonate and ferric chloride in the medium of water at a molar ratio of their respective 9:38:18. Get the product in the form of a fine crystalline powder, which is intended for use in medicine as substances with cardioprotective properties.

From RU 2073005 known way to obtain a chelate compound of a metal selected from the group of Cd, Cr, Fe, Bi, Mn, Zn, Sn, interaction chelat forming compounds of a certain formula, for example, 1-oxa-4,7,10-triazacyclononane-N,N',N"-trioxanes acid (or its salts) with a metal oxide or metal salt in the presence of, if necessary, hydroxide of alkaline metal. The resulting chelates metals are used as contrast agents for diagnostic in vivo Il the in vitro or in preparations or as a drug for radiotherapy.

From RU 2179162, C1, 10.02.2002 a method of obtaining of complexions metals (chelation), used to obtain solutions containing trace elements (Microvit"), including two chelating inorganic salts of metals using a combination of the two chelating agents in acidic environment: with citric acid, which serves as acidifying agent; and a secondary ligand in the complex formation with the participation of eddc (oksietilidendifosfonovaya acid). Eddc - complexing agents, active in an acidic environment.

One of the main factors affecting the complexation is the pH value of the solution: depending on the metal ion pH ranges in values of 1.5 to 2.3 or 2.4 to 3.5.

This drug is a complex of chelated metals (trace elements) in the optimal combination (except iron) with the addition of nitrogen and potassium components of essential nutrients. This combination is very effective against leaf nutrition of plants.

However, iron plants require several times more than it is contained in the "Microsite", so it is necessary to make, separately from other elements. Fully balanced combination of all the micronutrients, including iron, to prepare for this scheme is not possible, since Fe is an antagonist to copper and other components.

As a result of implementation of the method according to this known invention receive nutrient solution (concentrate trace elements)containing, g/l: Fe - 30, Mn - 30, B - 11, Zn - 8, Cu - 8, SB - 3, Mod - 5, Mg - 20, the nutrient solution of 1.35-1.45 g/cm3pH of 2.7-3.

From SU 492060, 09.08.1976 a method of obtaining of complexions metals (particularly iron) - chelate metal derived ethylenediaminetetraacetic acid specific structural formula (derived by the interaction of the anhydride of ethylenediaminetetraacetic acid with the amine R-NH2where R is the residue of a phenyl or naphthyl). Get chelates interaction above is derived from a combination of heavy metal, for example, ferric chloride, in the presence of water or alkanols, and hydroxides of alkali metals or ammonium.

Get, for example, chelates iron content of iron in concentrations of 0.3-10 mg of iron per 1 liter; pH support of 7.5-8. Depending on the addition of solid or liquid carrier receive (food) drugs in the form of solid preparations, in the form of concentrates of metal chelates, dispersible in water - wettable powder; in the form of liquid preparations of solutions in suitable organic solvents, and water. Solutions containing active start (chelates metals) at a concentration of 1-20. This known method does not receive chelation of iron with a high content of iron.

The closest in technical essence and the achieved result is known a method of obtaining a solution of a chelate of iron content in the final solution of iron up to 3-5%.

A method of obtaining the solution of the chelate iron polimeropeschanoj acid, comprising adding a salt of an alkali metal (sodium or potassium) polimeropeschanoj acid to aqueous iron salt solution (iron nitrate, iron chloride, iron sulfate, iron acetate), in terms of obtaining a stable solution: process temperature 5-100°With; the molar ratio of ligand and iron in the final product from 1.05:1 to 1.3:1; the pH of the solution of the alkali metal and polimeropeschanoj acid 8-14; pH of a solution of iron salts 0-4; pH of the final product 3-8. The resulting chelate iron can be used in agriculture, but is primarily intended for use in the photographic industry (US 5717123, 10.02.1998).

The technical objective of the claimed invention to provide a highly concentrated solution of a chelate of iron with a high content of iron in solution.

The goal of the project is achieved in that in the method of obtaining a concentrated solution of iron chelate interaction when mixed in water Sol the iron complexing agent when heated receive a concentrated aqueous solution of a chelate of iron with an iron content of 60-100 g/l, as the complexing agent used is N,N,N1N1- ethylenediaminetetraacetic acid and citric acid, which is administered simultaneously or sequentially; the process is carried out at 70-90°when mixed aqueous solution of iron salts in aqueous medium with a complexing agent, or after the mixture is injected into the reaction solution, an aqueous solution of ammonia or ammonium citrate to obtain a final product with a pH of 2.0 to 2.3. As salts of iron using iron sulfate, iron nitrate, iron chloride, iron acetate in aqueous solution or in dry form. In the process of complexing agent may further comprise succinic acid from 20 to 50 g/l

The object of the invention is also chelate iron in the form of a concentrated aqueous solution with a content of iron of 60-100 g/l, obtained stated above.

So, the problem to be solved by the present invention is directed, is a way of creating a separate highly concentrated solution of iron chelate for additional power plants, preventing chlorosis, and increase the concentration of iron in solution compared to, in particular, with the "Microvita".

The method is as follows. For example, hot water is injected citric acid and add ammonia solution until polucheniem solution of 1.5 to 2.5. Then enter the iron salt such as ferric sulfate, with the greatest affinity for citric acid under such conditions, conduct stirring until dissolved iron salts. Then add the second combined - EDTA to obtain a mixed-ligand complexant iron. Stirring is continued for 2-3 hours for education for sustainable connection.

The temperature of the dissolution of iron salts and the formation of chelates support in the range of 70-90°C. reduction slows down the reaction between the ingredients, and the increase in over 90°With undesirable because it will result in removal (evaporation) of ammonia and water and lower the pH below the optimal level.

As ammoniagenesis component in addition to ammonia, you can use the ammonium citrate, which in sufficient quantity plays the role of alkalizing agent, and is also a ligand for complexing agents citric acid, while the dosage of citric acid decrease.

The method is illustrated by the following examples without limiting the invention.

Example 1. In 500 ml of hot water is added (1.3 mol) in 250 g of citric acid, and then 80 ml of ammonia solution (25%) is stirred constantly, the temperature is kept 90°C, the pH of the solution is 2.0 to 2.3. Then add 500 grams of FeSO4·7H2(1.8 mol), stirred on the complete dissolution of the salt, then add 100 g (0.3 mol) of EDTA. The mixing process continued for 3 hours, which is necessary to complete complexation in solution. The result is mixed ligand chelate iron containing (1.8 mol) of 100 g/l Fe, density 1290 g/l In the final product the molar ratio of iron, citric acid and EDTA defined as

Fe: [citric acid + EDTA]=1,1:1

The initial molar ratio of the salt of iron: [citric acid + EDTA]=1,4:1 (L.K. - citric acid).

Example 2. The process is carried out, as shown in example 1, but the dosage of the following components:

- citric acid - 190 g (1.0 mol)

- ammonia solution (25%) - 55 ml

- EDTA - 70 g (0.2 mol)

- FeSO4·7H2About 350 g (1.25 mol)

Get solution of iron chelate containing 70 g/l Fe density of 1240 g/l

In the final product ratio is defined as

Fe: [citric acid + EDTA]=1,05:1

The initial molar ratio:

salt of iron: [citric acid + EDTA]=1,4:1.

Example 3. In 500 ml of hot water add complexing agent: 140 g of citric acid (0.7 mol) and 40 g (0.1 mol) EDTA, mix and then add 300 g of ferrous sulfate (FeSO4·7H2O), continuously stirred, the temperature of the support 75°S; pH of the solution is 2.1.

Next, in the obtained solution was added aqueous ammonia (25%) or citrate is ammonium in number, necessary to bring the pH of the final solution of the chelate iron.

Get solution of iron chelate, containing 60 g/l of iron, the density of 1220 g/l (1.0 mol). The molar ratio defined end (product):

Fe: [L.K. + EDTA]=1,0:0,8[mol]=1,25:1;

Source - Sol iron: [L.K. + EDTA]=300 g: 180 g = 1,6:1.

Example 4. The process is carried out similarly as in examples 1 or 3, but part of citric acid (L.K.) substituted succinic acid (AC), i.e. the use of citric acid in a quantity of 150 g/l (0.8 mol) and succinic acid in the amount of 30 g/l (0.25 mol), and the ratio between them of 3.2:1 (in moles).

Get solution of iron chelate containing 80 g/l (1,4 mole) of iron, the density of the solution 1275 g/cm3. In the final product ratio

Fe: [L.K. + AK + EDTA]=1,4:1,15=1,2:1.

The initial molar ratio is

salt of iron: [L.K. + AK + EDTA]=400 g: 230 g = 1,7:1.

Received stated the way the iron chelate is used as a top dressing (power) plants. Below is a specific example showing its use in this capacity. This drug is given the name "Perovic".

Application

Spraying of plants in the morning or evening hours with an aqueous solution of Farovite in a ratio of 1.5 ml per 1 liter of water.

Prophylactically with an interval of 10-14 days. To correct chlorosis 3-4 times a week.

Example 5. Regular spraying of plants working is m solution of Farovite (1.5 ml per 1 liter of water) 2-3 times in the spring. For complete wetting plant leaves the solution flow rate is 1 l 5-7 m2landing. Chlorosis of leaves is completely absent, there are strong flowering and fruiting berry bushes.

Example 6. When the first signs of chlorosis in tomato (pale green top) must be carried out by spraying the plants with a solution of Farovite (1.5 ml per 1 liter of water) every other day during the week. By the end of the week chlorosis fully removed.

1 l = 113 mg Fe/1 liter of solution.

1. The method of obtaining a concentrated solution of iron chelate interaction when mixed in an aqueous medium salts of iron complexing agent when heated, characterized in that get concentrated aqueous solution of a chelate of iron with an iron content of 60-100 g/l, as a complexing agent used is N,N,N',N'-ethylenediaminetetraacetic acid and citric acid, which is administered simultaneously or sequentially, the process is carried out at 70-90°With, in the process of mixing or after mixing of salt with iron complexing agent is added an aqueous solution of ammonia or ammonium citrate to achieve the pH of the final product 2,0-2,3.

2. The method according to claim 1, characterized in that as salts of iron using iron nitrate, iron sulfate, iron acetate.

3. The method according to claim 1 or 2, characterized in that complexarray is a first agent further comprises succinic acid.

4. The iron chelate in the form of a concentrated aqueous solution with an iron content of 60-100 g/l obtained by the method according to one of claims 1 to 3.



 

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SUBSTANCE: invention relates to the improved method for preparing metal complex compounds, in particular, to iron complex (chelate) as its concentrated solution. Method is carried out by interaction of iron salt in an aqueous medium with a chelate-forming agent wherein N,N,N',N'-ethylenediaminetetraacetic acid is used as a chelating agent and citric acid that are added simultaneously or successively. The process is carried out at temperature 70-90°C and in the process of mixing iron salt or after mixing with chelate-forming agent an aqueous solution of ammonia or ammonium citrate is added for providing pH value of the end product 2.0-2.3. The complex-forming agent can comprise succinic acid additionally. Method provides preparing iron chelate as a concentrated solution with the content of iron 60-100 g/l. Invention can be used in agriculture for root and leaf feeding of plants.

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6 cl, 7 ex

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36 cl, 1 dwg, 3 ex

FIELD: chemistry.

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EFFECT: disclosed method improves output of radioactive fluorination.

5 cl, 43 ex, 5 tbl, 6 dwg

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