CS229253B1 - A method of producing industrial liquid fertilizer - Google Patents

Abstract

The invention relates to a method for producing an industrial liquid fertilizer containing nitrogen bound in the form of a tertiary amine by reacting aqueous solutions and/or suspensions containing ammonium ions, wherein the aqueous solutions and/or suspensions containing ammonium ions react with aqueous solutions of formaldehyde in an amount corresponding to 0.67 to 25 moles, preferably 0.67 to 13.4 moles of ammonium per 1 mole of formaldehyde at a temperature of 20 to 80 °C, preferably 35 to 50 °C, wherein the reaction mixture is further reacted with 0.30 to 0.75 moles, preferably 0.33 to 0.67 moles of a basic reacting substance or a mixture of these substances. The basic reacting substance is gaseous ammonia, or its aqueous solution and/or ammonium carbonate and/or potassium hydroxide, and/or sodium hydroxide and/or potassium carbonate and/or sodium carbonate and/or sodium bicarbonate and/or potassium bicarbonate and/or magnesium oxide and/or magnesium carbonate and/or magnesium hydroxide and/or calcium oxide and/or calcium hydroxide and/or calcium carbonate.

Description

229253 3

BACKGROUND OF THE INVENTION The present invention relates to a process for the production of industrial liquid fertilizers comprising nitrogen in the form of a tertiary amine.

Nitrogen is a nutrient nutrient in plant nutrition, an indispensable structural element of every protein, and an irreplaceable macro-nutrient in chlorophyll formation. Nitrogen-containing industrial solid and liquid fertilizers may be present as ammoniacal and / or nitric and / or amide.

For example, ammoniacal and nitrate nitrogen contain cast iron; Ammonia (ammonium ammonium nitrate) from liquid fertilizers; ammoniacal, nitrate, and amide nitrogen include, for example, liquid UAN; "DAM-390" a. I.

The most common and at the same time the most concentrated fertilizer containing only ammonia nitrogen is liquid ammonia (82.2% N), which is also the most important starting material in the production of nitrogen-containing industrial fertilizers such as quarries; urea; ammonia; polyphosphoric fertilizers and other multi-component liquid and solution and suspension fertilizers.

Liquid ammonia, due to its high vapor pressure, is referred to as a pressurized nitrogen fertilizer, the distribution and application of which is relatively demanding.

For example, ammonia water is used from nitrogen-containing medium-pressure or non-pressurized liquid fertilizers; ammonium ammonium nitrate solution and urea; liquid nitrogen-phosphoric fertilizer based on orthophosphates or polyphosphates, as well as combinations of these fertilizers.

Urea is used for direct fertilization as a solid mono-constituent fertilizer containing 46.2% amide nitrogen, or as a liquid fertilizer in the form of its ammonia solution or in the form of non-pressurized liquid nitrogen fertilizer in combination with ammonium nitrate, known under the trade name "UAN" "(USA) or" DAM-390 "(CSSR). Slowly nitrogen-bearing fertilizers (e.g., "Ureafiorm") have a significant position among nitrogen-containing fertilizers, producing sufficient soil in the soil for the entire growing cycle; loss of nitrogen applied in this form. Most of the nitrogen-containing industrial fertilizers mentioned in the ammoniacal and / or nitrate and / or amide form are produced by energy-consuming and process-technological processes.

It has now been found that an industrial fertilizer comprising a portion of nitrogen in the form of a non-ionic tertiary amine compound according to the invention can be relatively easily prepared for the process equipment and the energy consumption.

The invention is based on the fact that the aqueous solutions and / or suspensions containing ammonium ion are reacted with an aqueous solution of formaldehyde in an amount corresponding to 0.67 to 25 mol, preferably 0.67 to 13.4 mol, of ammonium per mole of formaldehyde at ambient temperature. The reaction mixture is further reacted with 0.30 to 0.75 mol, preferably 0.33 to 0.67 mol, of the reactant or mixture thereof. As the basic reactant, ammonia gas or its aqueous solution and / or ammonium carbonate and / or potassium hydroxide and / or sodium hydroxide and / or potassium carbonate and / or sodium carbonate and / or sodium bicarbonate and / or potassium hydrogen carbonate and / or magnesium carbonate and / or magnesium carbonate and / or magnesium hydroxide and / or calcium oxide and / or calcium hydroxide and / or calcium carbonate.

The method of preparing the fertilizer industry according to the invention has the most advantageous advantage in that the fast-loving ammoniacal nitrogen is converted to a slow-acting nitrogen present in the form of tertiary amine. Furthermore, it is also possible to produce fertilizers containing, in addition to traditional forms of nitrogen (ammoniacal, urea), which are easily leachable, fertilizers suitable for storage manure, providing plants with sufficient nitrogen throughout the growing cycle. It is believed that due to the nonionic nature of the hexamethylenetetramine, the nitrogen bonded in this form is not subject to nitrification processes, the fertilizer prepared by the process of the invention may be in liquid (solution, suspension) or solid form, and can be applied to the granular in liquid form fertilizers, or used as one of the ingredients in the production of fertilizers. The process of the invention can be used to produce solid granular multi-component fertilizers containing an ammonium salt by administering an aqueous solution of formaldehyde and a base (e.g. MgCCb; technical MgO and the like) to the granulation mixture. Based on the preliminary results of the use of nitrogen-containing substances in the form of a non-ionic compound on the base of the plant nutrient amine, it can be assumed that this form of nitrogen, in comparison with ammoniacal, nitrate and amidic nitrogen, acts as a loosening nitrogen. The examples which follow illustrate, but do not limit, the invention. Example 1

Into a three-necked flask with a stirrer and a control thermometer, 66 parts by weight of crystalline ammonium sulfate, 170 parts by volume of distilled water and 121.27 229253 were introduced.

With parts by weight of a 37% aqueous solution of farmaldehyde. After stirring for 30 minutes, 24.42 parts by weight of so-called "soft burned" brick was added to the solution containing: 54.5% by weight of Mg

1.46% by weight Ca3.77% by weight Fe0.47% by weight Al

Total alkalinity: 223.93 ml 0.2 N H2SO4 per 1 g sample. The reaction mixture was stirred for 4 hours and after which time the suspension was filtered through a sintered glass sinter. The obtained filtrate contained 3.21% Mg (5.306% MgO), 3.62% nitrogen in the form of tertiary amine and 4.48% S.

Clarification point: -9.3 ° C. Example 2

A procedure analogous to Example 1. A solution is prepared: 59.68 parts by weight of NH 4 NO 3, 5.79 parts by weight of Ca (NO 3) 2.4 H 2 O, 7.79 parts by weight of Mg (NO 3) 2.6 H 2 O, 26.75 parts by weight of water to which 90.92 is used % by weight of 37% formaldehyde.

After stirring for 30 minutes, 16.5 parts by weight of technical MgO, the so-called "macaque burnt bricks" (specified in Example 1) are added.

The solution (filtrate) contains: 5.241% by weight Mg (8.63% MgO), 11.49% by weight total nitrogen, of which 6.01% N in the form of nitrate, 5.48% N in the form of tertiary amine, 0.51% Ca .

3.89.44 parts by weight of NH3NO3 98.5% by weight are mixed with 16.32 parts by weight of 37% formaldehyde while stirring, and 3.96 parts by weight are gradually added to this reaction mixture with continued stirring. dolomite (54% CaCO3 + 46% MgCO3), while releasing the released nitric acid. The reaction mixture is kept under stirring at room temperature for about 30 to 60 minutes, after which it is granulated in a known manner. The fertilizer obtained has the following composition: 15.4% ammonia N, 1.88% amine N, 16.55% total nitrate N, 33.83% total N, 1.2% CaO, 0.87% MgO, 0.50% H2O. Example 4

To the mixture of 36.56 parts by weight of triple sulfonate (45.5% by weight P2O5 dissolved in citric acid, 12% by weight H2O) and 38.82 parts by weight of KCl (60% by weight K2O) were added to the granulation apparatus62.97 parts by weight. of the reaction product obtained by the reaction of 25.92 parts by weight of ammoniacal nitric ammonium solution (20% by weight NH3, 63% by weight NH4NO3, 17% by weight H2O) with 37.05 parts by weight of 37% formaldehyde. After granules and drying, multi-component manure granules were obtained containing: 4.26% by weight amine nitrogen, 2.86% by weight ammonia, 2.86% by weight nitrate, 9.98% by weight total, 16.63% by weight of P2O5 dissolved in citric acid, 23.39% K2O, 2% H2O.

Claims (2)

SUBJECT 1. A process for producing a nitrogen-containing industrial liquid fertilizer bound in the form of a tertiary amine by reaction of aqueous solutions and / or suspensions! containing ammonium ions with an aqueous formaldehyde solution, characterized in that aqueous solutions and / or suspensions containing ammonium ions are reacted with an aqueous formaldehyde solution in an amount corresponding to 0.67 to 25 moles, preferably 0.67 to 13.4 moles of ammonium per mole of formaldehyde at a temperature of 20 to 80 ° C, preferably 35 to 50 ° C, wherein the reaction mixture is further reacted with 0.30 to 0.75 moles, preferably 0.33 to 0.67 moles. . Method according to claim 1, characterized in that the basic reacting substance is ammonia gas or an aqueous solution thereof and / or ammonium carbonate and / or potassium hydroxide and / or sodium hydroxide and / or potassium carbonate and / or sodium carbonate and / or or sodium bicarbonate and / or potassium bicarbonate and / or magnesium oxide and / or magnesium carbonate and / or magnesium hydroxide and / or calcium oxide and / or calcium hydroxide and / or calcium carbonate.