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 PDFInfo
- 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
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- exchange
- solution
- anion
- nitrate
- exchange membrane
- Prior art date
Links
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 23
- 235000010333 potassium nitrate Nutrition 0.000 title claims abstract description 17
- 239000004323 potassium nitrate Substances 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 238000000909 electrodialysis Methods 0.000 title claims abstract description 9
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 32
- 239000012528 membrane Substances 0.000 claims abstract description 31
- 239000003011 anion exchange membrane Substances 0.000 claims abstract description 28
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000005341 cation exchange Methods 0.000 claims abstract description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 16
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 16
- 239000001103 potassium chloride Substances 0.000 claims abstract description 16
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 16
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 12
- 239000000047 product Substances 0.000 claims abstract description 12
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000010344 sodium nitrate Nutrition 0.000 claims abstract description 11
- 239000004317 sodium nitrate Substances 0.000 claims abstract description 11
- 150000002500 ions Chemical class 0.000 claims abstract description 10
- 239000003014 ion exchange membrane Substances 0.000 claims abstract description 9
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011780 sodium chloride Substances 0.000 claims abstract description 8
- 239000006227 byproduct Substances 0.000 claims abstract description 7
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- 230000005684 electric field Effects 0.000 claims abstract description 3
- 235000002639 sodium chloride Nutrition 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 4
- 235000011167 hydrochloric acid Nutrition 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 125000006850 spacer group Chemical group 0.000 claims description 2
- 238000002955 isolation Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001805 chlorine compounds Chemical class 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 230000002572 peristaltic effect Effects 0.000 description 2
- 230000000750 progressive effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005816 glass manufacturing process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 230000009972 noncorrosive effect Effects 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000000606 toothpaste Substances 0.000 description 1
Classifications
-
- 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.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Water Supply & Treatment (AREA)
- Agronomy & Crop Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Urology & Nephrology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Water Treatment By Electricity Or Magnetism (AREA)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CZ2013-234A CZ304507B6 (cs) | 2013-03-28 | 2013-03-28 | Způsob výroby dusičnanu draselného metodou elektrodialýzy a zařízení k provádění tohoto způsobu |
| CZPV2013-234 | 2013-03-28 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2014154189A1 true WO2014154189A1 (en) | 2014-10-02 |
Family
ID=50687223
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/CZ2014/000030 WO2014154189A1 (en) | 2013-03-28 | 2014-03-21 | A method of production of potassium nitrate by electrodialysis and apparatus for making the same |
Country Status (2)
| Country | Link |
|---|---|
| CZ (1) | CZ304507B6 (cs) |
| WO (1) | WO2014154189A1 (cs) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104261435A (zh) * | 2014-10-10 | 2015-01-07 | 山东诺贝丰化学有限公司 | 一种复分解法硝酸钾结晶系统及结晶工艺 |
| CN112723390A (zh) * | 2021-02-03 | 2021-04-30 | 浙江艺谛环境设备有限公司 | 一种氯化钠与碳酸氢铵制备碳酸氢钠与氯化铵的处理系统及工艺 |
Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4465568A (en) | 1981-11-16 | 1984-08-14 | Olin Corporation | Electrochemical production of KNO3 /NaNO3 salt mixture |
| 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 |
| CN1122793A (zh) | 1994-11-05 | 1996-05-22 | 张辉 | 副产氮钾二元复合肥的生产方法 |
| CN1184077A (zh) | 1996-12-06 | 1998-06-10 | 陈淑奇 | 离子交换法生产硝酸钾工艺 |
| 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 |
| CN1827526A (zh) | 2005-08-31 | 2006-09-06 | 东华工程科技股份有限公司 | 一种复分解法制备硝酸钾的方法 |
| CN101628723A (zh) | 2009-08-18 | 2010-01-20 | 湖南丹化农资有限公司 | 复分解反应生产硝酸钾和氯化铵的方法 |
| CN101973564A (zh) | 2010-11-01 | 2011-02-16 | 赵家春 | 烟花爆竹用硝酸钾及其制备方法 |
| EP2418171A1 (en) * | 2006-01-06 | 2012-02-15 | Nextchem | Method for increasing the hydroxide content of polymetal hydroxychlorides used as antiperspirant salt compositions with enhanced efficacy |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4253929A (en) * | 1980-03-05 | 1981-03-03 | Philip Morris Incorporated | Method for denitration of tobacco employing electrodialysis |
| CH677325A5 (cs) * | 1989-04-28 | 1991-05-15 | Asea Brown Boveri | |
| JP3198297B2 (ja) * | 1992-11-27 | 2001-08-13 | 経済産業省産業技術総合研究所長 | 苛性ソーダの製造方法 |
| JP5072477B2 (ja) * | 2007-08-10 | 2012-11-14 | 株式会社アストム | 硝フッ酸廃液からの酸の回収方法 |
-
2013
- 2013-03-28 CZ CZ2013-234A patent/CZ304507B6/cs not_active IP Right Cessation
-
2014
- 2014-03-21 WO PCT/CZ2014/000030 patent/WO2014154189A1/en active Application Filing
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4465568A (en) | 1981-11-16 | 1984-08-14 | Olin Corporation | Electrochemical production of KNO3 /NaNO3 salt mixture |
| 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 |
| CN1122793A (zh) | 1994-11-05 | 1996-05-22 | 张辉 | 副产氮钾二元复合肥的生产方法 |
| CN1184077A (zh) | 1996-12-06 | 1998-06-10 | 陈淑奇 | 离子交换法生产硝酸钾工艺 |
| 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 |
| CN1827526A (zh) | 2005-08-31 | 2006-09-06 | 东华工程科技股份有限公司 | 一种复分解法制备硝酸钾的方法 |
| EP2418171A1 (en) * | 2006-01-06 | 2012-02-15 | Nextchem | Method for increasing the hydroxide content of polymetal hydroxychlorides used as antiperspirant salt compositions with enhanced efficacy |
| CN101628723A (zh) | 2009-08-18 | 2010-01-20 | 湖南丹化农资有限公司 | 复分解反应生产硝酸钾和氯化铵的方法 |
| CN101973564A (zh) | 2010-11-01 | 2011-02-16 | 赵家春 | 烟花爆竹用硝酸钾及其制备方法 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104261435A (zh) * | 2014-10-10 | 2015-01-07 | 山东诺贝丰化学有限公司 | 一种复分解法硝酸钾结晶系统及结晶工艺 |
| CN104261435B (zh) * | 2014-10-10 | 2015-12-02 | 诺贝丰（中国）化学有限公司 | 一种复分解法硝酸钾结晶系统及结晶工艺 |
| CN112723390A (zh) * | 2021-02-03 | 2021-04-30 | 浙江艺谛环境设备有限公司 | 一种氯化钠与碳酸氢铵制备碳酸氢钠与氯化铵的处理系统及工艺 |
Also Published As
| Publication number | Publication date |
|---|---|
| CZ2013234A3 (cs) | 2014-06-04 |
| CZ304507B6 (cs) | 2014-06-04 |
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