WO2014154189A1 - A method of production of potassium nitrate by electrodialysis and apparatus for making the same - Google Patents

A method of production of potassium nitrate by electrodialysis and apparatus for making the same Download PDF

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Publication number
WO2014154189A1
WO2014154189A1 PCT/CZ2014/000030 CZ2014000030W WO2014154189A1 WO 2014154189 A1 WO2014154189 A1 WO 2014154189A1 CZ 2014000030 W CZ2014000030 W CZ 2014000030W WO 2014154189 A1 WO2014154189 A1 WO 2014154189A1
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Prior art keywords
exchange
solution
anion
nitrate
exchange membrane
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PCT/CZ2014/000030
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French (fr)
Inventor
Lubomir MACHUCA
Ales CERNÍN
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Membrain S.R.O.
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Publication of WO2014154189A1 publication Critical patent/WO2014154189A1/en

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D9/00—Nitrates of sodium, potassium or alkali metals in general
    • C01D9/08—Preparation by double decomposition
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/42—Electrodialysis; Electro-osmosis ; Electro-ultrafiltration; Membrane capacitive deionization
    • B01D61/44—Ion-selective electrodialysis
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/42—Electrodialysis; Electro-osmosis ; Electro-ultrafiltration; Membrane capacitive deionization
    • B01D61/44—Ion-selective electrodialysis
    • B01D61/46—Apparatus therefor
    • B01D61/50—Stacks of the plate-and-frame type
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D9/00—Nitrates of sodium, potassium or alkali metals in general
    • C01D9/08—Preparation by double decomposition
    • C01D9/10—Preparation by double decomposition with ammonium nitrate
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D9/00—Nitrates of sodium, potassium or alkali metals in general
    • C01D9/08—Preparation by double decomposition
    • C01D9/14—Preparation by double decomposition of salts of potassium with sodium nitrate
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2313/00—Details relating to membrane modules or apparatus
    • B01D2313/14—Specific spacers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2313/00—Details relating to membrane modules or apparatus
    • B01D2313/28—Specific concentration chambers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2313/00—Details relating to membrane modules or apparatus
    • B01D2313/30—Specific dilution or de-ionizing chambers

Definitions

  • the invention concerns a method of production of potassium nitrate by means of electrodialysis, consisting in the exchange of ions between solution of potassium chloride and solution of ammonium nitrate, nitric acid or sodium nitrate.
  • the invention also concerns a apparatus to perform this method.
  • the produced potassium nitrate has a wide range of use: in agriculture as a fertilizer, in glassmaking and in production of explosives and pyrotechnics, in food-processing industry as a preservative or in pharmacy as an ingredient in toothpastes.
  • KN0 3 Potassium nitrate
  • NaN0 3 sodium nitrate
  • HN0 3 nitric acid
  • NNLN0 3 ammonium nitrate
  • the method of production of potassium nitrate by means of electrodialysis contributes to resolving these disadvantages while keeping the progressive features of the electrolytic process.
  • the principle of the invention consists in the fact that the exchange of ions between solution of potassium chloride and solution of ammonium nitrate, nitric acid or sodium nitrate occurs in electric field in a system of ion-exchange membranes, containing at least one sequence of anion-exchange membranes and cation-exchange membranes, alternating and creating at least four intermembrane spaces.
  • solutions of the said chemical compounds flow in the following manner: solution of input potassium chloride flows in the first intermembrane space before the first anion- exchange membrane; solution of ammonium nitrate, nitric acid or sodium nitrate flows in the third intermembrane space between the first cation-exchange membrane and the second anion-exchange membrane.
  • Solution of the main product - potassium nitrate - flows in the fourth intermembrane space between the second anion-exchange membrane and the second cation-exchange membrane, and solution of by-product - ammonium chloride, hydrochloric acid or sodium chloride - flows in the second intermembrane space between the first anion- exchange membrane and the first cation-exchange membrane.
  • the concentrations of input solutions of potassium chloride and ammonium nitrate, nitric acid or sodium nitrate should be between 0.01 and 0.3 mol/L, and the concentration of output solutions of products - potassium nitrate and ammonium chloride, hydrochloric acid or sodium chloride - is higher than 1 mol/L.
  • the operating temperature of solutions should range between 10 and 80 °C, preferably between 20 and 50 °C.
  • the device to perform the method according to the invention consists of electrodes, between which there is a system of ion-exchange membranes, containing at least one sequence of anion-exchange membranes and cation-exchange membranes, alternating and creating at least four intermembrane spaces (CI, C2, Dl, D2) for solutions of input and output chemical compounds of the dialytic exchange of ions.
  • Ion-exchange membranes should be of a homogeneous or heterogeneous type with the thickness of 0.1 to 1 mm and permselectivity of more than 90%, and between them there are spacers with the thickness of 0.1 to 2 mm, made of polymeric material to secure distribution and mutual non-mixing of solutions, and mechanical support of intermembrane spaces.
  • the voltage between electrodes should range between 0.5 to 2 V on the sequence of four membranes - membrane quadruplet - with current density from 40 to 400 A/m 2 .
  • Advantages of the method of obtaining potassium nitrate according to the invention consist in getting a highly purified K O 3 solution with a high level of conversion.
  • the conversion itself occurs in the device of electrodialyser, made of noncorrosive components based on polymeric materials.
  • Fig. 1 shows the functional scheme of the method of production of potassium nitrate by means of electrodialysis on one (basic) sequence of ion-exchange membranes
  • Fig. 2 shows an example of arrangement of five sequences of four membranes - membrane quadruplets.
  • the laboratory unit P EDR-Z/4x (by the MemBrain company) for electrodialysis- metathesis was used (hereafter only EDM).
  • the unit contained 5 tanks with the volumes from 0.25 to 2 litres and 5 centrifugal pumps with magnetic inserts for circulation of solution in intermembrane spaces CI , C2, D_i, D2, created by sequences of anion-exchange membranes AMI, AM2 and cation-exchange membranes CM1, CM2 (for a scheme of one basic sequence, see Fig. 1).
  • these were the following solutions: • diluate 1 - solution of input potassium chloride (KC1), flowing through the first intermembrane space Dl before the first anion-exchange membrane AMI,
  • the unit was equipped with tools to measure flow rates, temperature, conductivity and pH for each individual circuit and with direct current supply with the output of 90 W.
  • the EDM module was equipped with 11 cation-exchange membranes CM (RALEX CM-PES) and 10 anion-exchange membranes AM (RALEX AM-PES), alternating and creating 5 sequences of membranes (quadruplets) - see the scheme in Fig. 2. Each of these sequences was arranged according to Fig. 1. The effective area of one membrane was 64 cm 2 .
  • the test was performed analogously and on a device similar to Example 1, but in a continuous manner with recycling (feed and bleed).
  • the testing unit was supplemented with 2 external tanks for concentrated solutions of KCl and NH 4 N0 3 and 2 peristaltic pumps. Suction of peristaltic pumps was from the external tanks and outlet was connected to working circuits of KCl or ⁇
  • solution of KCl was added with concentration 0.2 mol L.
  • NH 4 N0 3 third intermembrane space D2 with concentration 0.03 mol/L
  • solution of ⁇ 3 ⁇ 4 ⁇ 0 3 was added with concentration 0.2 mol/L.

Abstract

The invention concerns a method of production of potassium nitrate by means of electrodialysis, consisting in the exchange of ions between solution of potassium chloride and solution of ammonium nitrate, nitric acid or sodium nitrate. This exchange of ions occurs in electric field in a system of ion-exchange membranes (see Figure 1), containing at least one sequence of anion-exchange membranes (AM1, AM2) and cation-exchange membranes (CM1, CM2), alternating and creating at least four intermembrane spaces (C1, C2, D1, D2). In these intermembrane spaces on both sides of membranes, solutions of the said chemical compounds flow in the following manner: solution of input potassium chloride flows in the first interaiembrane space (D1) before the first anion-exchange membrane; solution of ammonium nitrate, nitric acid or sodium nitrate flows in the third intermembrane space (D2) between the first cation-exchange membrane (CM1) and the second anion-exchange membrane; while solution of the main product - potassium nitrate - flows in the fourth intermembrane space (C2) between the second anion-exchange membrane (AM2) and the second cation-exchange membrane (CM2), and solution of by-product - ammonium chloride, hydrochloric acid or sodium chloride - flows in the second intermembrane space (C1) between the first anion-exchange membrane (AMI) and the first cation-exchange membrane (CM1). The invention also concerns an apparatus to perform this method.

Description

A METHOD OF PRODUCTION OF POTASSIUM NITRATE BY ELECTRODIALYSIS AND APPARATUS FOR MAKING THE SAME
Technology field
The invention concerns a method of production of potassium nitrate by means of electrodialysis, consisting in the exchange of ions between solution of potassium chloride and solution of ammonium nitrate, nitric acid or sodium nitrate. The invention also concerns a apparatus to perform this method. The produced potassium nitrate has a wide range of use: in agriculture as a fertilizer, in glassmaking and in production of explosives and pyrotechnics, in food-processing industry as a preservative or in pharmacy as an ingredient in toothpastes.
State of the art
Potassium nitrate (KN03) is produced by reaction of potassium chloride with one of the following substances: sodium nitrate (NaN03), nitric acid (HN03) or ammonium nitrate (NFLN03). Reactions follow these equations:
KC1 + NTLj Os -> KN03 + NH4CI
KC1 + HNO3 -= KN03 + HC1
KC1 + NaN03 -> KN03 + NaCl
At present, two main methods of synthesis are known:
1. Conversion in reactor: Solutions of compounds according to the equations above are mixed in a reactor where they react and the product - KN03 - coagulates in controlled heating/cooling. Such solutions are depicted e.g. in Chinese patents 1122793, 1827526, 101628723 or 101973564. Disadvantages of this method are low level of conversion, formation of sediments on the surface of the reactor in crystallization and high demands on the material of the reactor with respect to corrosive and chemical resistance.
2. By means of ion-exchangers: The exchange of cations is performed in a column with acid cation-exchanger - see e.g. Chinese patent 1184077, Canadian patent 2027064, European patent 1235743. After the exchange of ions, a solution is obtained, and to get a solid product, evaporation and crystallization always follow. A disadvantage of this method is getting KN03 solution with low concentration, which increases expenses for evaporation. In solutions according to U.S. patents 4465568 and US4995950, the exchange of ions occurs during electrodialysis. The driving force is direct current and a cation-exchange membrane is placed in the device for electrodialysis. Thanks to electrolysis, hydroxides KOH/NaOH are produced first, which react with H 03 to produce a mixture of nitrates N03/Na 03. Byproducts are gases, chlorine and hydrogen. The process of electrolytic production of potassium nitrate is a progressive technology with clear advantages over the described traditional production processes. However, the main disadvantage of this method is the fact that the product (KN03) is not produced directly but in subsequent neutralization. It also must be mentioned that the productivity of the process is not optimum.
Principle of the invention
The method of production of potassium nitrate by means of electrodialysis contributes to resolving these disadvantages while keeping the progressive features of the electrolytic process. The principle of the invention consists in the fact that the exchange of ions between solution of potassium chloride and solution of ammonium nitrate, nitric acid or sodium nitrate occurs in electric field in a system of ion-exchange membranes, containing at least one sequence of anion-exchange membranes and cation-exchange membranes, alternating and creating at least four intermembrane spaces. In these intermembrane spaces on both sides of membranes, solutions of the said chemical compounds flow in the following manner: solution of input potassium chloride flows in the first intermembrane space before the first anion- exchange membrane; solution of ammonium nitrate, nitric acid or sodium nitrate flows in the third intermembrane space between the first cation-exchange membrane and the second anion-exchange membrane. Solution of the main product - potassium nitrate - flows in the fourth intermembrane space between the second anion-exchange membrane and the second cation-exchange membrane, and solution of by-product - ammonium chloride, hydrochloric acid or sodium chloride - flows in the second intermembrane space between the first anion- exchange membrane and the first cation-exchange membrane.
The concentrations of input solutions of potassium chloride and ammonium nitrate, nitric acid or sodium nitrate, should be between 0.01 and 0.3 mol/L, and the concentration of output solutions of products - potassium nitrate and ammonium chloride, hydrochloric acid or sodium chloride - is higher than 1 mol/L. The operating temperature of solutions should range between 10 and 80 °C, preferably between 20 and 50 °C. The device to perform the method according to the invention consists of electrodes, between which there is a system of ion-exchange membranes, containing at least one sequence of anion-exchange membranes and cation-exchange membranes, alternating and creating at least four intermembrane spaces (CI, C2, Dl, D2) for solutions of input and output chemical compounds of the dialytic exchange of ions. Ion-exchange membranes should be of a homogeneous or heterogeneous type with the thickness of 0.1 to 1 mm and permselectivity of more than 90%, and between them there are spacers with the thickness of 0.1 to 2 mm, made of polymeric material to secure distribution and mutual non-mixing of solutions, and mechanical support of intermembrane spaces.
The voltage between electrodes should range between 0.5 to 2 V on the sequence of four membranes - membrane quadruplet - with current density from 40 to 400 A/m2.
Advantages of the method of obtaining potassium nitrate according to the invention consist in getting a highly purified K O3 solution with a high level of conversion. The conversion itself occurs in the device of electrodialyser, made of noncorrosive components based on polymeric materials.
Overview of figures in drawings
The principle of the technical solution can be clarified by the attached drawing, in which Fig. 1 shows the functional scheme of the method of production of potassium nitrate by means of electrodialysis on one (basic) sequence of ion-exchange membranes and Fig. 2 shows an example of arrangement of five sequences of four membranes - membrane quadruplets.
Examples of implementation of the invention Example 1
For testing, the laboratory unit P EDR-Z/4x (by the MemBrain company) for electrodialysis- metathesis was used (hereafter only EDM). The unit contained 5 tanks with the volumes from 0.25 to 2 litres and 5 centrifugal pumps with magnetic inserts for circulation of solution in intermembrane spaces CI , C2, D_i, D2, created by sequences of anion-exchange membranes AMI, AM2 and cation-exchange membranes CM1, CM2 (for a scheme of one basic sequence, see Fig. 1). Specifically, these were the following solutions: • diluate 1 - solution of input potassium chloride (KC1), flowing through the first intermembrane space Dl before the first anion-exchange membrane AMI,
• diluate 2 - solution of input ammonium nitrate (NH4NO3), nitric acid (HN03) or sodium nitrate (NaN03), flowing through the third intermembrane space D2 between the first cation-exchange membrane CM1 and the second anion-exchange membrane AM2,
• concentrate 1 - solution of the main product - potassium nitrate (KNO3) - flowing through the fourth intermembrane space C2 between the second anion-exchange membrane AM2 and the second cation-exchange membrane CM2,
• concentrate 2 - solution of by-product - ammonium chloride (NH4CI), hydrochloric acid (HC1) or sodium chloride (NaCl) - flowing through the second intermembrane space CI between the first ion-exchange membrane AMI and the first cation-exchange membrane CM1.
• electrode solution.
The unit was equipped with tools to measure flow rates, temperature, conductivity and pH for each individual circuit and with direct current supply with the output of 90 W. The EDM module was equipped with 11 cation-exchange membranes CM (RALEX CM-PES) and 10 anion-exchange membranes AM (RALEX AM-PES), alternating and creating 5 sequences of membranes (quadruplets) - see the scheme in Fig. 2. Each of these sequences was arranged according to Fig. 1. The effective area of one membrane was 64 cm2.
The test was performed in the batch method. Input solutions were processed of KC1 - first intermembrane space D_I, volume 1 litre, concentration 0.2 mol/L - and of NH NO3 - third intermembrane space D2, volume 1 litre, concentration 0.2 mol/L.
Solutions circulated through the EDM module at the speed of 0.5 L/min and their temperature was 25 °C. The operating voltage was 7.5 V and the current dropped from 2.5 A to 1.7 A at the end of the experiment. By this method, 50 mL of the main product KNO3 were produced - fourth intermembrane space C2 with concentration 4 mol/L - and 50 mL of by-product NH4CI - second intermembrane space CI with concentration 2.8 mol/L. The content of chlorides in the main product was 2 mol.%. Throughout the experiment, solution of NH4NO3 with concentration 0.3 mol/L was flowing in the electrode chambers.
Example 2
The test was performed analogously and on a device similar to Example 1, but in a continuous manner with recycling (feed and bleed). The testing unit was supplemented with 2 external tanks for concentrated solutions of KCl and NH4N03 and 2 peristaltic pumps. Suction of peristaltic pumps was from the external tanks and outlet was connected to working circuits of KCl or ΝΗφΝίΟ^ To the processed solution of KCl (first intermembrane space Dl) with concentration 0.03 mol/L, solution of KCl was added with concentration 0.2 mol L. To the processed solution of NH4N03 (third intermembrane space D2) with concentration 0.03 mol/L, solution of Ι¾Ν03 was added with concentration 0.2 mol/L. The speed of adding these solutions was controlled to keep the constant concentration of solutions at 0.03 mol/L. The circulation speed of solutions through the EDM module was 0.5 L/min. At the temperature of 25 °C and voltage of 7.5 V , the constant current was 1.3 A. By processing 1.5 litre of solution of KCl with 0.2 mol/L and 1.5 litre of solution of H4 03 with 0.2 mol/L was produced 100 ml of the main product K O3 (fourth intermembrane space C2) with concentration 3 mol L and 100 ml of by-product NH4CI (second mtermembrarie space CI) with concentration 2.7 mol/L. The content of chlorides in the main product was 2 mol.%. Throughout the experiment, solution of NH4N03 with concentration 0.2 mol/L was flowing in the electrode chambers.

Claims

C L A I M S
1. A method of production of potassium nitrate by electrodialysis, consisting in the exchange of ions between solution of potassium chloride and solution of ammonium nitrate, nitric acid or sodium nitrate, with possible subsequent isolation of potassium nitrate from the solution, characterized in that this exchange of ions occurs in electric field in a system of ion-exchange membranes, containing at least one sequence of anion-exchange membranes (AMI, AM2) and cation-exchange membranes (CM1, CM2), alternating and creating at least four intermembrane spaces (CI, C2, Dl, D2), in these intermembrane spaces (CI, C2, Dl, D2) on both sides of membranes (AMI, AM2, CM1, CM2), solutions of the said chemical compounds flow in the following manner: solution of input potassium chloride flows in the first intermembrane space (Dl) before the first anion-exchange membrane; solution of ammonium nitrate, nitric acid or sodium nitrate flows in the third intermembrane space (D2) between the first cation-exchange membrane (CM1) and the second anion-exchange membrane; while solution of the main product - potassium nitrate - flows in the fourth intermembrane space (C2) between the second anion-exchange membrane (AM2) and the second cation-exchange membrane (CM2), and solution of byproduct - ammonium chloride, hydrochloric acid or sodium chloride - flows in the second intermembrane space (CI) between the first anion-exchange membrane (AMI) and the first cation-exchange membrane (CM1).
2. The method according to Claim 1, characterized in that the concentrations of input solutions of potassium chloride and ammonium nitrate, nitric acid or sodium nitrate, ranging between 0.01 and 0.3 mol/L, and by the concentration of output solutions of products - potassium nitrate and ammonium chloride, hydrochloric acid or sodium chloride - higher than 1 mol/L.
3. The method according to Claim 1, characterized in that the operating temperature of solutions, ranging between 10 and 80 °C, preferably between 20 and 50 °C.
4. An apparatus to perform the method according to Claim 1, characterized in that it consists of electrodes, between which there is a system of ion-exchange membranes, containing at least one sequence of anion-exchange membranes (AMI, AM2) and cation-exchange membranes (CM1, CM2), alternating and creating at least four intermembrane spaces (CI, C2, Dl, D2) for solutions of input and output chemical compounds of the dialytic exchange of ions, with ion-exchange membranes being of a homogeneous or heterogeneous type with the thickness of 0.1 to 1 mm and permselectivity of more than 90%, between which there are spacers with the thickness of 0.1 to 2 mm, made of polymeric material to secure distribution and mutual non-mixing of solutions, and mechanical support of intermembrane spaces.
5. The apparatus according to Claim 4, characterized in that the voltage between electrodes ranging between 0.5 to 2 V on the sequence of four membranes - membrane quadruplet - and current density of 40 to 400 A/m2.
PCT/CZ2014/000030 2013-03-28 2014-03-21 A method of production of potassium nitrate by electrodialysis and apparatus for making the same WO2014154189A1 (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104261435A (en) * 2014-10-10 2015-01-07 山东诺贝丰化学有限公司 Potassium nitrate crystallization system and process through double-decomposition method
CN112723390A (en) * 2021-02-03 2021-04-30 浙江艺谛环境设备有限公司 Processing system and process for preparing sodium bicarbonate and ammonium chloride from sodium chloride and ammonium bicarbonate

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WO1986006646A1 (en) * 1985-05-03 1986-11-20 Allied Corporation Recovery of mixed acids from mixed salts
US4995950A (en) 1987-09-04 1991-02-26 Basf Aktiengesellschaft Preparation of alkali metal nitrates
CA2027064A1 (en) 1989-10-05 1991-04-06 Alvaro Abidaud Continuous production of potassium nitrate via ion exchange
US5110578A (en) * 1989-10-05 1992-05-05 Monomeros Colombo Venezolanos, S.A. (E.M.A.) Continuous production of potassium nitrate via ion exchange
US5207879A (en) * 1991-03-11 1993-05-04 The Graver Company Bipolar membrane stack and method for production of low chloride sodium hydroxide
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EP1235743A1 (en) 1999-12-03 2002-09-04 Kemira Agro Oy Production of two alkali metal salts by a combined ion exchange and crystallisation process
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CN101628723A (en) 2009-08-18 2010-01-20 湖南丹化农资有限公司 Method for preparing potassium nitrate and ammonium chloride employing double decomposition reaction
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104261435A (en) * 2014-10-10 2015-01-07 山东诺贝丰化学有限公司 Potassium nitrate crystallization system and process through double-decomposition method
CN104261435B (en) * 2014-10-10 2015-12-02 诺贝丰（中国）化学有限公司 A kind of double decomposition potassium nitrate crystal system and crystallization processes
CN112723390A (en) * 2021-02-03 2021-04-30 浙江艺谛环境设备有限公司 Processing system and process for preparing sodium bicarbonate and ammonium chloride from sodium chloride and ammonium bicarbonate

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