CN107162023A - The preparation system and preparation method of a kind of potassium nitrate - Google Patents

The preparation system and preparation method of a kind of potassium nitrate Download PDF

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Publication number
CN107162023A
CN107162023A CN201710376982.8A CN201710376982A CN107162023A CN 107162023 A CN107162023 A CN 107162023A CN 201710376982 A CN201710376982 A CN 201710376982A CN 107162023 A CN107162023 A CN 107162023A
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salt
salt room
salting liquid
room
solution
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韩效钊
严勋
张旭
汪小尧
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Hefei University of Technology
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Hefei University of Technology
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Priority to CN201710376982.8A priority Critical patent/CN107162023A/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
    • C01D9/14—Preparation by double decomposition of salts of potassium with sodium 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
    • C01D9/10—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
    • C01D9/12—Preparation by double decomposition with nitrates or magnesium, calcium, strontium, or barium
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05C—NITROGENOUS FERTILISERS
    • C05C1/00—Ammonium nitrate fertilisers

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Agronomy & Crop Science (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The invention discloses a kind of preparation system of potassium nitrate and preparation method, wherein：System includes electrodialysis membrane stack and is fixed on the positive and negative electrode of electrodialysis membrane stack both sides；By cation-exchange membrane and anion-exchange membrane, alternate intervals are arranged electrodialysis membrane stack successively, form anode chamber, cathode chamber, the first salt room, the second salt room, the 3rd salt room and the 4th salt room；During preparation, potassium nitrate, nitrate, chlorate and Klorvess Liquid are separately added into four salt rooms, open dc source, nitrate ion in second salt room is moved in the first salt room under electric field action by anion-exchange membrane, potassium ion in 4th salt room is moved in the first salt room under electric field action by cation-exchange membrane, and now potassium ion combines in the first salt room with nitrate ion and obtains potassium nitrate.Present invention process flow is simple, can continuously produce, and whole process is carried out at normal temperatures, small to equipment corrosion, and energy consumption is low, non-secondary pollution, low in raw material price.

Description

The preparation system and preparation method of a kind of potassium nitrate
Technical field
The present invention relates to chlorideless potassic fertilizer production technical field, and in particular to a kind of use electrodialytic technique prepares potassium nitrate Device and method.
Background technology
Potassium nitrate is a kind of important without chlorine potassium, nitrogen composite fertilizer material, and nutrient for plants potassium, the total content of nitrogen are up to 50% left side The right side, is particularly suitable for use in the administration of some fear-chlorion crops, such as potassium nitrate, which is applied to tobacco, to be had high fertilizer efficiency, easy absorption, promote seedling Early send out, increase the advantage of tobacco production, to improving cigarette quality important role.China national standard GBT-20784-2013 is advised Fixed, the potassium nitrate of high-class product requires that potassium oxide mass fraction >=46.0%, chlorine ions fraction are less than 0.2% during agricultural is used, In addition total nitrogen content is less than 13.5%.
At present, the main technique of domestic production potassium nitrate has conversion method, ion-exchange, solvent extraction and double decomposition (Duan Zhengkang, Xie Fan, Zhang Tao, Li Sheng, Yan Jianhua, the problem of process for producing potassium nitrate general introduction and double decomposition are present and countermeasure, nothing Machine salt industrial, 2015,47 (5)：4-8.).
(1) conversion method：Using sodium nitrate (main component is sodium nitrate) and potassium chloride as the conversion method of raw material, reaction equation For：KCl+NaNO3→KNO3+NaCl.Potassium chloride dissolving and sodium nitrate in circulating mother liquor, first pass through evaporation, enrichment, centrifugation Isolated sodium chloride byproduct, then by the mother liquor of separation add water regulation concentration, crystallize through vacuum cooled, enrichment, centrifugation Temperature is obtained, the potassium nitrate product that can obtain technical grade is recrystallized finally by refining kettle.
(2) ion-exchange：Predominantly ammonium nitrate and potassium chloride ions exchange process, when the potassium ion in solution passes through ammonium type During ion exchange resin, occur exchange reaction with the ammonium ion in resin, be adsorption reaction, ion exchange resin is changed by ammonium type For potassium type, reaction equation is：RNH4+ KCl=RK+NH4Cl；When the ammonium ion in solution is by potassium type ion exchange resin, with tree Exchange reaction occurs for the potassium ion in fat, is elution of reactive, while ion exchange resin is changed into ammonium type from potassium type, reaction equation is： RK+NH4NO3=RNH4+KNO3.The potassium nitrate solution purity of method outflow is high, technological process is short, can operate continuously.Major defect It is that clearing house obtains that solution concentration is low, evaporation cost is high, equipment requirement is higher.
(3) solvent extraction：Solvent extraction can substantially be divided into 3 classes：Extracting HCl method, extraction KNO3Method, HCl and KNO3Point Other extraction.Israel is to be mainly used in industrial solvent extraction at present using the IMI methods of organic solvent extracting HCl, The technique is less likely to occur side reaction in the presence of low temperature and organic solvent, and by-product hydrochloric acid can be used for decomposing phosphate rock to produce phosphorus Acid.Reaction equation is：KCl+HNO3→KNO3+HCl。
(4) double decomposition：Double decomposition produces potassium nitrate and is divided into 2 kinds of non-round robin and round-robin method.(the Chen Wen such as Chen Wenwei Prestige, Lang little Chuan, iatreusiology product, the research of ammonium nitrate and KCl production potassium nitrate, applicable technology market, 2000, (2)：25-26) Potassium nitrate is prepared using double decomposition non-round robin, also can obtain nitrogenous, phosphorus, potassium etc. after the evaporation of addition phosphate fertilizer in remaining mother liquor contains The compound fertilizer of multiple element.Double decomposition circulation process is developed earliest by French Auby companies, and being divided into 3 steps again in technique follows Around-France and 4 one-step circulation methods.Most of China enterprise uses 4 one-step circulation method technique productions potassium nitrate.
In summary, easily limited compared to conversion method by resource, ion-exchange equipment cost is higher, solvent There is the risk of factory's blast in extraction, double decomposition has become the main method of domestic product potassium nitrate, but this method exists There are still potassium nitrate inferior separating effect, crystallisation by cooling rate be low, heat-transfer surface fouling is serious and impurity-eliminating effect is undesirable etc. in production Problem.
Although prior art can prepare the higher potassium nitrate product of quality, the process prepared is more or less deposited Economic benefit is low, complex process, pollution the problems such as.
The content of the invention
In view of this, the purpose of the present invention is to propose to a kind of preparation system of potassium nitrate and preparation method, using the present invention The system and method for offer prepare potassium nitrate, and technological process is simple, can operate continuously, investment cost is low, energy consumption is low, without secondary dirt Dye.
The invention provides a kind of preparation system of potassium nitrate, including：
Electrodialysis membrane stack, positive electrode, negative electrode, electrolyte sampling device, the first salting liquid generating means, the second salting liquid Sampling device, three-salt solution generating means, the 4th salting liquid sampling device, the first salting liquid storage device, the second salting liquid Storage device, three-salt solution storage device, the 4th salting liquid storage device, water storage apparatus and dc source；
The negative electrode is connected with the negative pole of the dc source；The positive pole phase of the positive electrode and the dc source Even；The negative electrode and the positive electrode are respectively arranged at the both sides of the electrodialysis membrane stack；
The electrodialysis membrane stack is internally formed cathode chamber, anode chamber, the first salt room, the second salt room, the 3rd salt room and the 4th The compartment of salt room six；
The outlet of the electrolyte sampling device is connected with the charging aperture of the anode chamber, the discharging opening of the anode chamber with The charging aperture of the cathode chamber is connected, and the import of the electrolyte sampling device is connected with the discharging opening of the cathode chamber, constitutes The circulation loop of electrolyte；
The outlet of the first salting liquid generating means is connected with the charging aperture of the first salt room, first salting liquid The import of generating means is connected with the discharging opening of the first salt room, constitutes the circulation loop of the first salting liquid；
The outlet of the second salting liquid sampling device is connected with the charging aperture of the second salt room, the second salt room Discharging opening is connected with the import of the second salting liquid storage device, the outlet of the second salting liquid storage device and described the The import of two salting liquid sampling devices is connected, and constitutes the circulation loop of the second salting liquid；
The outlet of the three-salt solution generating means is connected with the charging aperture of the 3rd salt room, the three-salt solution The import of generating means is connected with the discharging opening of the 3rd salt room, constitutes the circulation loop of three-salt solution；
The outlet of the 4th salting liquid sampling device is connected with the charging aperture of the 4th salt room, the 4th salt room Discharging opening is connected with the import of the 4th salting liquid storage device, the outlet of the 4th salting liquid storage device and described the The import of four salting liquid sampling devices is connected, and constitutes the circulation loop of the 4th salting liquid；
The outlet of the water storage apparatus respectively with the first salting liquid generating means, three-salt solution generating means Import is connected；
The import of the first salting liquid storage device and the outlet of the first salting liquid generating means pass through overflow manner phase Even；The import of the three-salt solution storage device is connected with the outlet of three-salt solution generating means by overflow manner.
It is preferred that, the electrodialysis membrane stack is arranged by cation-exchange membrane, filter and anion-exchange membrane successively alternate intervals Row are constituted, and close to positive electrode and negative electrode are cation-exchange membrane, between positive electrode and adjacent cation-exchange membrane Anode chamber is formed, cathode chamber is formed between negative electrode and adjacent cation-exchange membrane；Between anode chamber and cathode chamber by according to The cation-exchange membrane and anion-exchange membrane of secondary alternate intervals arrangement constitute one or more first salt rooms, the second salt room, the Three salt rooms and the repeat unit of the 4th salt room；
It is preferred that, the preparation system also includes clamping device, and the clamping device is used to fix the negative electrode, positive electricity Pole and electrodialysis membrane stack；
It is preferred that, it is real by interval of anion-exchange membrane between the first salt room and the second salt room inside the electrodialysis membrane stack Existing ion exchange, realizes ion exchange by interval of cation-exchange membrane between the second salt room and the 3rd salt room, the 3rd salt room with Between 4th salt room ion exchange is realized by interval of anion-exchange membrane；4th salt room and next repeat unit adjacent thereto The first salt room between realize ion exchange by interval of cation-exchange membrane.
Present invention also offers a kind of preparation method of potassium nitrate, it uses above-mentioned preparation system to carry out potassium nitrate system It is standby, comprise the following steps：
Strong electrolytic solution is transported in electrodialysis membrane stack anode chamber and cathode chamber by electrolyte sampling device；
Potassium nitrate solution is transported in the first salt of electrodialysis membrane stack room by the first salting liquid generating means, while by water Water in storage device is continually transported to certain flow in the first salting liquid generating means so that the first salting liquid is generated The first salting liquid is overflowed in the first salting liquid storage device in device；
Nitrate solution is transported in the second salt of electrodialysis membrane stack room by the second salting liquid sampling device；
Chlorination salting liquid is transported in the salt room of electrodialysis membrane stack the 3rd by three-salt solution generating means, while by water Water in storage device is continually transported in three-salt solution generating means with certain flow so that three-salt solution is generated Three-salt solution is overflowed in three-salt solution storage device in device；
Klorvess Liquid is transported in the salt room of electrodialysis membrane stack the 4th by the 4th salting liquid sampling device.
The nitrate ion for opening nitrate solution in dc source, the second salt room is handed under electric field action by anion Change film to move in the first salt room, the potassium ion in the 4th salt room in Klorvess Liquid passes through cation exchange under electric field action Film is moved in the first salt room, and now potassium ion combines in the first salt room with nitrate ion and obtains potassium nitrate.
It is preferred that, the one kind of the strong electrolytic solution in potassium hydroxide, sodium nitrate, potassium nitrate and ammonium nitrate solution Or several, most preferably potassium nitrate solution.
It is preferred that, the strong electrolytic solution concentration is 0.01~2mol/L.
It is preferred that, one or more of the chlorination salting liquid in ammonium chloride, sodium chloride and magnesium chloride solution are optimal Elect ammonium chloride solution as.
It is preferred that, it is 0.01~6.5mol/L to make chlorination concentration of salt solution in the 3rd salt room generating means.
It is preferred that, the molar concentration for making Klorvess Liquid in the 4th salting liquid sampling device is saturation molar concentration.
It is preferred that, one or more of the nitrate solution in ammonium nitrate, sodium nitrate and magnesium nitrate are most preferably Ammonium nitrate solution.
It is preferred that, it is 0.01~3mol/L to make potassium nitrate solution concentration in the first salt room generating means.
It is preferred that, the molar concentration for making nitrate solution in the second salting liquid sampling device is saturation molar concentration.
Compared with prior art, beneficial effects of the present invention are embodied in：
Preparation system and method that the present invention is provided, using nitrate as the supply source of nitrate ion, pass through cation Being used alternatingly for exchange membrane and anion-exchange membrane, potassium nitrate is changed into by potassium chloride, and product purity is high, technological process is simple, It is easily achieved mechanization, serialization and automation；And whole process can be carried out at normal temperatures, raw material small to equipment corrosion Wide material sources, energy consumption is low, cheap, non-secondary pollution.
Brief description of the drawings
Fig. 1 is the structural representation of potassium nitrate preparation system provided in an embodiment of the present invention, in figure：1 is dc source, 2 It is the negative pole of dc source for the positive pole of dc source, 3,4 be positive electrode, and 5 be negative electrode, and 6 be the first salt room tank, and 7 be the 3rd Salt room tank, 8 be the second salt room tank, and 9 be the second salt room surge tank, and 10 be the 4th salt room tank, and 11 be the 4th salt room surge tank, and 12 are Electrolyte is filled, and 13 be deionized water holding vessel, and 14 and 15 be peristaltic pump, and 16 and 17 be clamping device, and 18 be electrodialysis membrane stack, 19 It is the 3rd salt room immersible pump for the first salt room immersible pump, 20,21 be the second salt room immersible pump, and 22 be the 4th salt room immersible pump, 23 It is the charging aperture of anode chamber for electrolyte immersible pump, 24,25 be the discharging opening of cathode chamber, and 26 be the charging aperture of the first salt room, 27 It is the charging aperture of the 3rd salt room for the discharging opening of the first salt room, 28,29 be the discharging opening of the 3rd salt room, 30 entering for the second salt room Material mouth, 31 be the discharging opening of the second salt room, and 32 be the charging aperture of the 4th salt room, and 33 be the discharging opening of the 4th salt room, and 34 be first Salt room product overflow receiving tank, 35 be the 3rd salt room product overflow receiving tank, and 36 be electrodialytic membranes stack device.
Fig. 2 is the internal structure schematic diagram of electrodialysis membrane stack in potassium nitrate preparation system provided in an embodiment of the present invention, its In 37 be anion-exchange membrane, 38,39 composition filters；40 be cation-exchange membrane, and 41 be filter.42nd, 43 be respectively illustrate it is molten Liquid enters outgoing direction.
Fig. 3 is the electrodialysis membrane stack voltage versus time curve figure of 1~embodiment of the embodiment of the present invention 3.
Embodiment
The preparation system for the potassium nitrate that the present invention is provided, including：
Electrodialysis membrane stack, positive electrode, negative electrode, electrolyte sampling device, the first salting liquid generating means, the second salting liquid Sampling device, three-salt solution generating means, the 4th salting liquid sampling device, the first salting liquid storage device, the second salting liquid Storage device, three-salt solution storage device, the 4th salting liquid storage device, water storage apparatus and dc source；
The negative electrode is connected with the negative pole of the dc source；The positive pole phase of the positive electrode and the dc source Even；The negative electrode and the positive electrode are respectively arranged at the both sides of the electrodialysis membrane stack；
The electrodialysis membrane stack is internally formed cathode chamber, anode chamber, the first salt room, the second salt room, the 3rd salt room and the 4th The compartment of salt room six；
The outlet of the electrolyte sampling device is connected with the charging aperture of the anode chamber, the discharging opening of the anode chamber with The charging aperture of the cathode chamber is connected, and the import of the electrolyte sampling device is connected with the discharging opening of the cathode chamber, constitutes The circulation loop of electrolyte；
The outlet of the first salting liquid generating means is connected with the charging aperture of the first salt room, first salting liquid The import of generating means is connected with the discharging opening of the first salt room, constitutes the circulation loop of the first salting liquid；
The outlet of the second salting liquid sampling device is connected with the charging aperture of the second salt room, the second salt room Discharging opening is connected with the import of the second salting liquid storage device, the outlet of the second salting liquid storage device and described the The import of two salting liquid sampling devices is connected, and constitutes the circulation loop of the second salting liquid；
The outlet of the three-salt solution generating means is connected with the charging aperture of the 3rd salt room, the three-salt solution The import of generating means is connected with the discharging opening of the 3rd salt room, constitutes the circulation loop of three-salt solution；
The outlet of the 4th salting liquid sampling device is connected with the charging aperture of the 4th salt room, the 4th salt room Discharging opening is connected with the import of the 4th salting liquid storage device, the outlet of the 4th salting liquid storage device and described the The import of four salting liquid sampling devices is connected, and constitutes the circulation loop of the 4th salting liquid；
The outlet of the water storage apparatus respectively with the first salting liquid generating means, three-salt solution generating means Import is connected；
The import of the first salting liquid storage device and the outlet of the first salting liquid generating means pass through overflow manner phase Even；The import of the three-salt solution storage device is connected with the outlet of three-salt solution generating means by overflow manner.
Fig. 1 is the structural representation of potassium nitrate preparation system provided in an embodiment of the present invention, in figure：1 is dc source, 2 It is the negative pole of dc source for the positive pole of dc source, 3,4 be positive electrode, and 5 be negative electrode, and 6 be the first salt room tank, and 7 be the 3rd Salt room tank, 8 be the second salt room tank, and 9 be the second salt room surge tank, and 10 be the 4th salt room tank, and 11 be the 4th salt room surge tank, and 12 are Electrolyte is filled, and 13 be deionized water holding vessel, and 14 and 15 be peristaltic pump, and 16 and 17 be clamping device, and 18 be electrodialysis membrane stack, 19 It is the 3rd salt room immersible pump for the first salt room immersible pump, 20,21 be the second salt room immersible pump, and 22 be the 4th salt room immersible pump, 23 It is the charging aperture of anode chamber for electrolyte immersible pump, 24,25 be the discharging opening of cathode chamber, and 26 be the charging aperture of the first salt room, 27 It is the charging aperture of the 3rd salt room for the discharging opening of the first salt room, 28,29 be the discharging opening of the 3rd salt room, 30 entering for the second salt room Material mouth, 31 be the discharging opening of the second salt room, and 32 be the charging aperture of the 4th salt room, and 33 be the discharging opening of the 4th salt room, and 34 be first Salt room product overflow receiving tank, 35 be the 3rd salt room product overflow receiving tank, and 36 be electrodialytic membranes stack device.
In the present invention, the preparation system of potassium nitrate includes electrodialysis membrane stack.Electrodialysis membrane stack include anion-exchange membrane, Cation-exchange membrane and filter, the filter are located between anion-exchange membrane and cation-exchange membrane.The present invention is to described the moon Amberplex and cation-exchange membrane do not have special limitation, using cation-exchange membrane well known to those skilled in the art and Anion-exchange membrane, is bought by market and obtained.In an embodiment of the present invention, the anion-exchange membrane, cation are handed over Every effective area for changing film can be 5cm2~400cm2；In a further embodiment, the anion-exchange membrane, cation are handed over Change the every effective area or 10cm of film2~200cm2；In other examples, the anion-exchange membrane, cation Every effective area of exchange membrane can also be 20cm2.What the present invention can be provided using Shandong Tianwei Membrane Technology Co., Ltd. Anion-exchange membrane and cation-exchange membrane.
In the present invention, the cation-exchange membrane, filter, anion-exchange membrane, filter, cation-exchange membrane order are folded Constitute repeat unit after pressure, and close to positive electrode and negative electrode be cation-exchange membrane, positive electrode and adjacent cation Anode chamber is formed between exchange membrane, cathode chamber is formed between negative electrode and adjacent cation-exchange membrane；In anode chamber and negative electrode The cation-exchange membrane and anion-exchange membrane arranged between room by alternate intervals successively constitutes one or more first salt rooms, the The repeat unit of disalt room, the 3rd salt room and the 4th salt room.In an embodiment of the present invention, the electrodialysis membrane stack can include 1~20 repeat unit.
In the present invention, the repeat unit preferably also includes sealing gasket, and the sealing gasket is arranged at the cation and handed over Change between film and the positive electricity pole plate, between the cation-exchange membrane and the negative electricity pole plate.
In the present invention, the edge of the filter preferably includes aperture, and the aperture includes sealed aperture and apertured orifice, The sealed aperture is used to cause liquid flowing；The opening direction of the apertured orifice is preferably filter middle part so that liquid can On the one hand to carry out ion exchange at middle part, on the other hand continued to flow out according to aperture direction, can be for control outlet port. Preferably also include aperture on the anion-exchange membrane and cation-exchange membrane, aperture is closed pores, and positioned at film edge. By the composition of above-mentioned film and aperture be set so that independent room each between can carry out ion exchange, and solely Each self-forming circulation loop and export controllable between vertical room.
In the present invention, the position relationship of the filter, anion-exchange membrane, cation-exchange membrane and aperture such as Fig. 2 institutes Show, be the electrodialysis membrane stack internal structure schematic diagram provided in an embodiment of the present invention for preparing potassium nitrate system, wherein 37 for it is cloudy from Proton exchange, 38,39 composition filters；40 be cation-exchange membrane, and 41 be filter.42nd, 43 be respectively that signal solution enters outgoing direction.
In the present invention, the negative electrode and the positive electrode are respectively placed in the both sides of the electrodialysis membrane stack.The present invention There is no special limitation to the negative electrode and positive electrode, using used in electrodialytic membranes stack device well known to those skilled in the art Negative electrode and positive electrode, meet practical operation condition.In the present invention, the negative electrode passes through wire and dc source Negative pole be connected；The positive electrode is connected by wire with the positive pole of dc source.In an embodiment of the present invention, the direct current Power supply be and the negative electrode and the supporting dc source of the positive electrode.
In the present invention, the clamping device is used to fix the negative electrode, positive electrode and electrodialysis membrane stack.The present invention is right The clamping device does not have special limitation, meets practical operation condition.In an embodiment of the present invention, it is described to clamp dress Putting can be made up of two pieces of clamping iron plates and bolt, and two pieces of clamping iron plates are respectively arranged to the both sides of the electrodialysis membrane stack, Blending bolt is fastened.
In the present invention, the electrodialysis membrane stack is internally formed anode chamber, cathode chamber, the first salt room, the second salt room, the 3rd Salt room and the compartment of the 4th salt room six.The outlet of the electrolyte sampling device is connected with the charging aperture of the anode chamber, described The discharging opening of anode chamber is connected with the charging aperture of the cathode chamber, import and the cathode chamber of the electrolyte sampling device Discharging opening is connected, and constitutes the circulation loop of electrolyte；In the present invention, the discharging opening of the cathode chamber is arranged on and anode chamber Discharging opening, the discharging opening of the first salt room, the discharging opening of the second salt room, the discharging opening of the 3rd salt room and the discharging opening of the 4th salt room are not Same position；The charging aperture of the cathode chamber is arranged on and the charging aperture, the charging aperture of the first salt room, the second salt room of anode chamber The different position of the charging aperture of charging aperture, the charging aperture of the 3rd salt room and the 4th salt room.In the present invention, the anode chamber is entered Material mouth is arranged on the charging aperture with cathode chamber, the charging aperture of the first salt room, the charging aperture of the second salt room, the charging aperture of the 3rd salt room The position different with the charging aperture of the 4th salt room；The discharging opening of the anode chamber is arranged on the discharging opening of cathode chamber, the first salt room Discharging opening, the discharging opening of the second salt room, the discharging opening of the 3rd salt the room position different with the discharging opening of the 4th salt room.The present invention In, the import of the electrolyte sampling device can be identical with the outlet of the electrolyte sampling device, can also be different.
In an embodiment of the present invention, circulating for the ease of electrolyte, the outlet of the electrolyte sampling device The first attachment means can be provided between the charging aperture of the anode chamber；The charging aperture of the cathode chamber and the anode chamber Discharging opening between can be provided with the second attachment means；The charging aperture of the electrolyte sampling device goes out with the cathode chamber The 3rd attachment means can be provided between material mouth.The present invention is filled to the first attachment means, the second attachment means and the 3rd connection Put without special limitation, meet practical operation condition；In an embodiment of the present invention, first attachment means can be with For emulsion tube；Second attachment means can be emulsion tube；3rd attachment means can be emulsion tube.
In the present invention, the electrolyte sampling device preferably includes electrolyte container and electrolyte conveying device. In the present invention, the import of the electrolyte container is connected with the discharging opening of the cathode chamber；The electrolyte conveying dress Install and be placed in inside the electrolyte container.In an embodiment of the present invention, the charging aperture of the electrolyte container It is connected with the discharging opening of the cathode chamber using the 3rd attachment means described in above-mentioned technical proposal；The electrolyte conveying device Outlet be connected using the first attachment means described in above-mentioned technical proposal with the charging aperture of the anode chamber；The anode chamber Discharging opening is connected using the second attachment means described in above-mentioned technical proposal with the charging aperture of the cathode chamber.
In the present invention, the electrolyte container is used to hold electrolyte.In the present invention, the electrolyte is preferred For strong electrolytic solution, more preferably strong electrolytic solution is in potassium hydroxide, sodium nitrate, potassium nitrate and ammonium nitrate solution One or more, most preferably potassium nitrate solution.In the present invention, the molar concentration of the electrolyte is preferably 0.01mol/L ~2mol/L, more preferably 0.03mol/L~1.5mol/L, most preferably 0.06mol/L~1.2mol/L, be the most preferably 0.08mol/L~1mol/L.The present invention does not have special limitation to shape, the material and size of the electrolyte container, Meet practical operation condition；In an embodiment of the present invention, electrolyte container can be electrolyte tank 12.
In the present invention, the electrolyte conveying device is used to the electrolyte in the electrolyte container being delivered to In the cathode chamber, electrolyte is delivered to the anode by the cathode chamber and the second attachment means of the anode chamber again Room, electrolyte is delivered to the electrolyte by the 3rd attachment means of the anode chamber and the electrolyte container again and contained Put in container, form circulation loop.In an embodiment of the present invention, electrolyte conveying device can be electrolyte immersible pump 23.
In the present invention, the outlet of the first salting liquid generating means is connected with the charging aperture of the first salt room, institute The import for stating the first salting liquid sampling device is connected with the discharging opening of the first salt room.In the present invention, the first salt room Charging aperture be arranged on the charging aperture of the anode chamber, the charging aperture of cathode chamber, the charging aperture of the second salt room, the 3rd salt room and enter The material mouth position different with the charging aperture of the 4th salt room；The discharging opening of the first salt room is arranged on the discharging of the anode chamber Mouth, the discharging opening of cathode chamber, the discharging opening of the second salt room, the discharging opening of the 3rd salt the room position different with the discharging opening of the 4th salt room Put.In the present invention, the outlet phase that the imports of the first salting liquid generating means can be with the first salting liquid generating means Together, can also be different.The present invention is by by the outlet of the first salting liquid generating means and the charging aperture of the first salt room It is connected, the import of the first salting liquid generating means is connected with the discharging opening of the first salt room so that the first salting liquid is given birth to Circulation loop is formed between the first salt room inside device and electrodialysis membrane stack.
In an embodiment of the present invention, circulating for the ease of the first salting liquid, the first salting liquid generation dress The 4th attachment means can be provided between the outlet put and the charging aperture of the first salt room；The discharging opening of the first salt room There can be the 5th attachment means between import with the first salting liquid generating means.The present invention is to the 4th attachment means There is no special limitation with the 5th attachment means, meet practical operation condition；In the present invention, the 4th attachment means Can be identical with the first attachment means described in above-mentioned technical proposal with the 5th attachment means, can also be different.The present invention's In embodiment, the 4th attachment means can be emulsion tube, and the 5th attachment means can be emulsion tube.
In the present invention, the first salting liquid generating means preferably include the first salting liquid container and the first salt is molten Liquid conveying device.In the present invention, the import of the first salting liquid container is connected with the discharging opening of the first salt room； The first salting liquid conveying device is arranged inside the first salting liquid container；In an embodiment of the present invention, institute The outlet of the first salting liquid conveying device is stated using the 4th attachment means described in above-mentioned technical proposal and the first salt room Charging aperture is connected；The import of the first salting liquid container is using the 5th attachment means described in above-mentioned technical proposal and institute The discharging opening for stating the first salt room is connected.
In the present invention, the outlet of the water storage apparatus is connected with the import of the first salt room solution container, The import of the first salting liquid storage device is connected with the outlet of the first salting liquid container by overflow manner.
In an embodiment of the present invention, the first salting liquid container is passed into for the ease of water then successively to prepare Product potassium nitrate, the outlet of the water storage apparatus can be provided with the 6th with the import of the first solution generating means and be connected Device and the first water conveying device；The present invention does not have special limitation to the 6th attachment means, meets practical operation condition ；In the present invention, the 6th attachment means can be identical with the first attachment means described in above-mentioned technical proposal, also may be used With difference.In an embodiment of the present invention, the 6th attachment means can be emulsion tube.In the present invention, first salting liquid Container is used to hold salting liquid, preferably potassium nitrate solution.In the present invention, the volume of the potassium nitrate solution is preferably just Well so that the first salt room solution container reaches overflow situation；The concentration of the potassium nitrate solution is preferably 0.01~3mol/ L, more preferably 0.3~3mol/L, most preferably 1~3mol/L, preferably the most 2~2.5mol/L.The present invention is to the first salt Shape, the material and size of solution container do not have special limitation, meet practical operation condition；In the reality of the present invention Apply in example, the first salting liquid container can be the first salt room tank 6.
In the present invention, the water storage apparatus is used to hold water.The volume of the water be preferably storage device 1/3~ 2/3.The present invention does not have special limitation to shape, the material and size of water storage apparatus, meets practical operation condition； In embodiments of the invention, water storage apparatus can be deionized water holding vessel 13.
In the present invention, the first salting liquid storage device goes out for holding the overflow from the first salting liquid container The salting liquid come.The present invention does not have special limitation to shape, the material and size of the first salting liquid storage device, meets actual Operating condition；In an embodiment of the present invention, the first salting liquid storage device can receive for the first salt room product overflow Tank 34.In the present invention, the first salting liquid conveying device is used for the first salt in the first salting liquid container Solution is delivered in the first salt room inside the electrodialysis membrane stack.In an embodiment of the present invention, first salting liquid is defeated It can be the first salt room immersible pump 19 to send device.
In the present invention, first water conveying device is used to the water in the water storage apparatus being delivered to described first Salting liquid is held in solution.In an embodiment of the present invention, first water conveying device can be peristaltic pump 14.
In the present invention, the outlet of the second salting liquid sampling device is connected with the charging aperture of the second salt room, institute The discharging opening for stating the second salt room is connected with the import of the second salting liquid storage device, the second salting liquid storage device Outlet is connected with the import of the second salting liquid sampling device so that inside the second salting liquid sampling device, electrodialysis membrane stack The second salt room, form circulation loop between the second salting liquid storage device.In the present invention, the second salting liquid sampling device Import can be identical with the outlet of the second salting liquid sampling device, can also be different.
In an embodiment of the present invention, circulating for the ease of salting liquid, the second salting liquid sampling device There can be the 7th attachment means between outlet and the charging aperture of the second salt room, the discharging opening of the second salt room and described the There can be the 8th attachment means between the import of disalt solution storage device, the outlet of the second salting liquid storage device and the There can be the 9th attachment means between the import of two salting liquid sampling devices.The present invention is filled to the 7th attachment means, the 8th connection Put, the 9th attachment means do not have special limitation, meet practical operation condition；In the present invention, the 7th attachment means, Eight attachment means, the 9th attachment means can be identical with the first attachment means described in above-mentioned technical proposal, can also be different. In embodiments of the invention, the 7th attachment means can be emulsion tube, and the 8th attachment means can be emulsion tube, the 9th connection dress It can be emulsion tube to put.
In the present invention, the second salting liquid sampling device preferably includes the second salting liquid container and the second salt is molten Liquid conveying device.In the present invention, the import of the second salting liquid container and the outlet of the second salting liquid storage device It is connected；The second salting liquid conveying device is arranged inside the second salting liquid container.In embodiments of the invention In, the import of the second salting liquid container and the outlet of the second salting liquid storage device are used described in above-mentioned technical proposal The 9th attachment means be connected；The import of the salting liquid storage device and the discharging opening of the second salt room use above-mentioned technical proposal The 8th described attachment means, the outlet of the charging aperture of the second salt room and the second salting liquid container uses above-mentioned technology The 7th attachment means described in scheme are connected.
In the present invention, the second salting liquid container is used to hold nitrate solution, preferably sodium nitrate, nitric acid One or more in magnesium and ammonium nitrate solution, most preferably ammonium nitrate solution.In the present invention, mole of the nitrate solution Concentration is saturation molar concentration.The present invention does not have special limitation to shape, the material and size of the second salting liquid container, Meet practical operation condition；In an embodiment of the present invention, the second salting liquid container can be the second salt room tank 8.
In the present invention, the second salting liquid storage device is used to hold nitrate solution and nitrate solid, is preferably One or more in sodium nitrate, magnesium nitrate and ammonium nitrate, most preferably ammonium nitrate.In the present invention, the nitrate solution is Saturated solution, the volume of the nitrate solution is preferably to be filled to the outlet of the second salting liquid storage device.The present invention is to the Shape, the material and size of disalt solution storage vessel do not have special limitation, meet practical operation condition；In the present invention Embodiment in, the second salting liquid storage device can be the second salt room surge tank 9.
In the present invention, the second salting liquid conveying device is used for second in the second salting liquid container Salting liquid is delivered in the second salt room inside electrodialysis membrane stack.In an embodiment of the present invention, the second salting liquid conveying device It can be the second salt room immersible pump 21.
In the present invention, the outlet of the three-salt solution generating means is connected with the charging aperture of the 3rd salt room, institute The import for stating three-salt solution sampling device is connected with the discharging opening of the 3rd salt room.In the present invention, the 3rd salt room Charging aperture be arranged on the charging aperture of the anode chamber, the charging aperture of cathode chamber, the charging aperture of the first salt room, the second salt room and enter The material mouth position different with the charging aperture of the 4th salt room；The discharging opening of the 3rd salt room is arranged on the discharging of the anode chamber Mouth, the discharging opening of cathode chamber, the discharging opening of the first salt room, the discharging opening of the second salt room position different with the discharging opening of the 4th salt room Put.In the present invention, the outlet phase that the imports of the three-salt solution generating means can be with the three-salt solution generating means Together, can also be different.The present invention is by by the outlet of the three-salt solution generating means and the charging aperture of the 3rd salt room It is connected, the import of the three-salt solution generating means is connected with the discharging opening of the 3rd salt room so that three-salt solution is given birth to Circulation loop is formed between the 3rd salt room inside device and electrodialysis membrane stack.
In an embodiment of the present invention, circulating for the ease of three-salt solution, the three-salt solution generation dress The tenth attachment means can be provided between the outlet put and the charging aperture of the 3rd salt room；The discharging opening of the 3rd salt room There can be the 11st attachment means between the charging aperture of the three-salt solution generating means.The present invention is connected to the described tenth Device and the 11st attachment means do not have special limitation, meet practical operation condition；In the present invention, the described tenth connects Connection device and the 11st attachment means can be identical with the first attachment means described in above-mentioned technical proposal, can also be different. In embodiments of the invention, the tenth attachment means can be emulsion tube, and the 11st attachment means can be emulsion tube.
In the present invention, the three-salt solution generating means preferably include three-salt solution container and the 3rd salt is molten Liquid conveying device.In the present invention, the import of the three-salt solution container is connected with the discharging opening of the 3rd salt room； The three-salt solution conveying device is arranged inside the three-salt solution container；In an embodiment of the present invention, institute The outlet of three-salt solution conveying device is stated using the tenth attachment means described in above-mentioned technical proposal and the 3rd salt room Charging aperture is connected；The import of the three-salt solution container using the 11st attachment means described in above-mentioned technical proposal with The discharging opening of the 3rd salt room is connected.
In the present invention, the outlet of the water storage apparatus is connected with the import of the three-salt solution container, institute The import for stating three-salt solution storage device is connected with the outlet of three-salt solution container by overflow manner.
In an embodiment of the present invention, three-salt solution container is passed into for the ease of water then successively to prepare Byproduct chlorate, the outlet and the import of the three-salt solution generating means of the water storage apparatus can be provided with the tenth Two attachment means and the second water conveying device；The present invention does not have special limitation to the 12nd attachment means, meets actual Operating condition；In the present invention, the 12nd attachment means can be connected dress with first described in above-mentioned technical proposal Put identical, can also be different.In an embodiment of the present invention, the 12nd attachment means can be emulsion tube.In the present invention, institute Stating three-salt solution container is used to hold salting liquid, preferably chlorination salting liquid, most preferably sodium chloride, magnesium chloride and chlorine Change the one or more in ammonium salt solution, most preferably ammonium chloride solution.In the present invention, the volume of the chlorination salting liquid is preferably Just so that reaching overflow situation in the 3rd salt room solution container；The concentration of the chlorination salting liquid is preferably 0.01~ 6.5mol/L, more preferably 0.3~6.5mol/L, most preferably 4~6.5mol/L, preferably the most 5~5.5mol/L.This hair Bright shape, material and size to three-salt solution container do not have special limitation, meet practical operation condition； In embodiments of the invention, three-salt solution container can be the first salt room tank 7.
In the present invention, the three-salt solution storage device goes out for holding the overflow from three-salt solution container The salting liquid come.The present invention does not have special limitation to shape, the material and size of three-salt solution storage device, meets actual Operating condition；In an embodiment of the present invention, three-salt solution storage device can receive for the 3rd salt room product overflow Tank 35.In the present invention, the three-salt solution conveying device is used for the 3rd salt in the three-salt solution container Solution is delivered in the 3rd salt room inside the electrodialysis membrane stack.In an embodiment of the present invention, the three-salt solution is defeated It can be the 3rd salt room immersible pump 20 to send device.
In the present invention, second water conveying device is used to the water in the water storage apparatus being delivered to the described 3rd In salting liquid container.In an embodiment of the present invention, second water conveying device can be peristaltic pump 15.
In the present invention, the outlet of the 4th salting liquid sampling device is connected with the charging aperture of the 4th salt room, institute The discharging opening for stating the 4th salt room is connected with the import of the 4th salting liquid storage device, the 4th salting liquid storage device Outlet is connected with the import of the 4th salting liquid sampling device so that inside the 4th salting liquid sampling device, electrodialysis membrane stack The 4th salt room, form circulation loop between the 4th salting liquid storage device.In the present invention, the 4th salting liquid sampling device Import can be identical with the outlet of the 4th salting liquid sampling device, can also be different.
In an embodiment of the present invention, circulating for the ease of salting liquid, the 4th salting liquid sampling device Can have the 13rd attachment means between outlet and the charging aperture of the 4th salt room, the discharging opening of the 4th salt room with it is described Can there are the 14th attachment means, the outlet of the 4th salting liquid storage device between the import of 4th salting liquid storage device There can be the 15th attachment means between import with the 4th salting liquid sampling device.The present invention is to the 13rd attachment means, the 14 attachment means, the 15th attachment means do not have special limitation, meet practical operation condition；In the present invention, 13 attachment means, the 14th attachment means, the 15th attachment means can be connected dress with first described in above-mentioned technical proposal Put identical, can also be different.In an embodiment of the present invention, the 13rd attachment means can be emulsion tube, the 14th connection dress It is emulsion tube to put, and the 15th attachment means can be emulsion tube.
In the present invention, the 4th salting liquid sampling device preferably includes the 4th salting liquid container and the 4th salt is molten Liquid conveying device.In the present invention, the import of the 4th salting liquid container and the outlet of the 4th salting liquid storage device It is connected；The 4th salting liquid conveying device is arranged inside the 4th salting liquid container.In embodiments of the invention In, the import of the 4th salting liquid container is with the outlet of the 4th salting liquid storage device using described in above-mentioned technical proposal The 15th attachment means be connected；The import of the 4th salting liquid storage device uses above-mentioned skill with the discharging opening of the 4th salt room The 14th attachment means described in art scheme, the outlet of the charging aperture and the 4th salting liquid container of the 4th salt room is used The 13rd attachment means described in above-mentioned technical proposal are connected.
In the present invention, the 4th salting liquid container is used to hold Klorvess Liquid.In the present invention, the chlorination The molar concentration of potassium solution is saturation molar concentration.The present invention does not have to shape, the material and size of the 4th salting liquid container There is special limitation, meet practical operation condition；In an embodiment of the present invention, the 4th salting liquid container can be 4th salt room tank 10.
In the present invention, the 4th salting liquid storage device is used to hold Klorvess Liquid and solid potassium chloride.The present invention In, the Klorvess Liquid is saturated solution, and the volume of the Klorvess Liquid is preferably to be filled to the 4th salting liquid storage dress The outlet put.The present invention does not have special limitation to shape, the material and size of the 4th salting liquid storage container, meets actual behaviour Make condition；In an embodiment of the present invention, the 4th salting liquid storage device can be the 4th salt room surge tank 11.
In the present invention, the 4th salting liquid conveying device is used for the 4th in the 4th salting liquid container Salting liquid is delivered in the 4th salt room inside electrodialysis membrane stack.In an embodiment of the present invention, the 4th salting liquid conveying device It can be the 4th salt room immersible pump 22.
In the present invention, it is preferred to carry out constant current or constant voltage operation to said apparatus using dc source 1.
Present invention also offers a kind of preparation method of potassium nitrate, using above-mentioned system, comprise the following steps：
Strong electrolytic solution is transported in electrodialysis membrane stack anode chamber and cathode chamber by electrolyte sampling device；
Potassium nitrate solution is transported in the first salt of electrodialysis membrane stack room by the first salting liquid generating means, while by water Water in storage device is continually transported to certain flow in the first salting liquid generating means so that the first salting liquid is generated The first salting liquid is overflowed in the first salting liquid storage device in device；
Nitrate solution is transported in the second salt of electrodialysis membrane stack room by the second salting liquid sampling device；
Chlorination salting liquid is transported in the salt room of electrodialysis membrane stack the 3rd by three-salt solution generating means, while by water Water in storage device is continually transported in three-salt solution generating means with certain flow so that three-salt solution is generated Three-salt solution is overflowed in three-salt solution storage device in device；
Klorvess Liquid is transported in the salt room of electrodialysis membrane stack the 4th by the 4th salting liquid sampling device.
Open dc source, in the second salt room the nitrate ion of nitrate solution under electric field action by the moon from Proton exchange is moved in the first salt room, and the potassium ion in the 4th salt room in Klorvess Liquid leads under electric field action Cross cation-exchange membrane to move in the first salt room, potassium ion is combined with nitrate ion in the first salt room obtains Potassium nitrate.
In the present invention, strong electrolytic solution is transported to electrodialysis membrane stack anode chamber by electrolyte sampling device first In cathode chamber；The strong electrolytic solution is preferably selected from one kind in potassium hydroxide, sodium nitrate, potassium nitrate and ammonium nitrate solution Or several, more preferably potassium nitrate solution.In the present invention, the molar concentration of the electrolyte is preferably 0.01~3mol/L, More preferably 0.3~3mol/L, most preferably 1~2mol/L, preferably the most 1.2~1.5mol/L.
The present invention has been clearly described for said apparatus and mode of movement, will not be repeated here.
In the present invention, above-mentioned electrolyte conveying device be used for provide power supply from electrolyte, have the chamber of circulation. Position relationship with remaining salt room can be without limiting.
In the present invention, it is the potassium nitrate solution in the first salting liquid container is defeated by the first salting liquid conveying device It is sent in the first salt room of electrodialysis membrane stack；The volume of the potassium nitrate solution is preferably to fill the first salting liquid container. In the present invention, the molar concentration of potassium nitrate solution is preferably 0.01~3mol/L, more preferably 0.3~3mol/L, most preferably For 1~3mol/L, preferably the most 2~2.5mol/L.
In the present invention, water is transported in the first salting liquid container by the first water conveying device.
In the present invention, the saturation nitrate solution in the second salting liquid container is conveyed by the second salting liquid and filled Put in the second salt room for being transported to electrodialysis membrane stack；The volume of the saturation nitrate solution is preferably to flood the second salting liquid Sheng Put the second salting liquid conveying device in container.
In the present invention, the saturation nitrate solution in the second salting liquid storage device is transported to by way of overflow In second salting liquid container；The volume of the saturation nitrate solution is preferably to flood the second salting liquid storage device.
In the present invention, the chlorination salting liquid in three-salt solution container is passed through into three-salt solution generation conveying dress Put in the 3rd salt room for being transported to electrodialysis membrane stack；The volume of the chlorination salting liquid is preferably to fill three-salt solution to hold appearance Device.In the present invention, the molar concentration of chlorination salting liquid is preferably 0.01~6.5mol/L, more preferably 0.3~6.5mol/L, Most preferably 4~6.5mol/L, preferably the most 5~5.5mol/L.
In the present invention, water is transported in three-salt solution container by the second water conveying device.
In the present invention, the saturated potassium chloride solution in the 4th salting liquid container is conveyed by the 4th salting liquid and filled Put in the 4th salt room for being transported to electrodialysis membrane stack；The volume of the saturated potassium chloride solution is preferably to flood the 4th salting liquid Sheng Put the 4th salting liquid conveying device in container.
In the present invention, the saturated potassium chloride solution in the 4th salting liquid storage device is transported to by way of overflow In 4th salting liquid container；The volume of the saturated potassium chloride solution is preferably to flood the 4th salting liquid storage device.
In the present invention, the saturation potassium chloride in the saturation nitrate solution and the 4th salt room in the second salt room Solution carries out ion exchange in electrodialysis membrane stack, obtains obtaining chlorate in potassium nitrate, the 3rd salt room in the first salt room.
In the present invention, it is preferred that before running gear so that solution circulation flow moves discharger inner air；Treat sky After gas discharge, dc source, running gear are opened.It is furthermore preferred that it is specially to open immersible pump that the solution circulation flow is dynamic so that The solution of anode chamber and cathode chamber, the first salt room, the second salt room, the 3rd salt room, the 4th salt room is each flowed by circulation loop.
To further appreciate that the present invention, the preparation system and method for the potassium nitrate provided with reference to embodiment the present invention It is described in detail, but they can not be interpreted as limiting the scope of the present invention.
Embodiment 1
Assemble preparation system：Specifically, electrodialytic membranes stack device 36 is replaced by anion-exchange membrane and cation-exchange membrane There are 11 pairs of anion-exchange membranes and cation-exchange membrane weight plus what the auxiliary materials such as runner filter and sealing gasket were constituted after laminating The electrodialysis membrane stack 18 that multiple unit is constituted, every effective area is 200cm2, and it is separately positioned on the moon at electrodialysis membrane stack two ends Electrode 5, positive electrode 4, and be placed in electrode two ends clamping device 16,17 constitute clamp what is formed by bolt.Repeat unit Put in order composition by materials described below：Filter, cation-exchange membrane, filter, anion-exchange membrane, filter, cation-exchange membrane； Cation-exchange membrane in repeat unit is close to positive electrode, and cation-exchange membrane is close to negative electrode；Clamping device include battery lead plate, Bolt, nut and pad.Above-mentioned part need to only be pressed Fig. 1 laminated structures by assembling electrodialysis membrane stack, then load onto electrodialysis Membrane stack clamping device 16,17, then screw up with a wrench.
The charging aperture 24 of the anode chamber of electrodialytic membranes stack device 36, the discharging opening 25 of cathode chamber, the charging aperture of the first salt room 26th, the discharging opening 27 of the first salt room, the charging aperture 30 of the second salt room, the discharging opening 31 of the second salt room, the charging aperture of the 3rd salt room 28th, the discharging opening 29 of the 3rd salt room, the charging aperture 32 of the 4th salt room, the discharging opening 33 of the 4th salt room are connected by emulsion tube respectively To corresponding electrode chamber tank 12, the first salt room tank 6, the second salt room surge tank 9, the 3rd salt room tank 7, the 4th salt room surge tank 11 Inside, the second salt room surge tank 9, the 4th salt room surge tank 11 are connected to the second salt room tank 8, the 4th salt room by emulsion tube respectively The inside of tank 10.Electrolyte fills the 12, first salt room tank 6, the second salt room tank 8, the 3rd salt room tank 7, put inside the 4th salt room tank 10 Have what is be connected respectively with corresponding electrode chamber, the first salt room, the second salt room, the 3rd salt room and the charging aperture emulsion tube of the 4th salt room Electrode chamber immersible pump 23, the first salt room immersible pump 19, the second salt room immersible pump 21, the 3rd salt room immersible pump 20 and the 4th salt room are latent Water pump 22, forms electrode chamber, the first salt room, the second salt room, the independent circulation loop in the 3rd salt room and the 4th salt room five；It will go Water in ion water store tank 13 is pumped into the first salt room tank 6, the 3rd salt room tank 7 by peristaltic pump 14,15 respectively；By the first salt room Tank 6, the 3rd salt room tank 7 are placed in the first salt room product overflow receiving tank 34, the 3rd salt room product overflow receiving tank 35；By the electricity The positive electrode 4 and negative electrode 5 of dialyser stack device 36 are connected by wire with the positive pole 2 and negative pole 3 of supporting dc source 1 respectively Connect.
Potassium nitrate is prepared using above-mentioned shown preparation system, comprised the following steps：
The potassium nitrate solution that 400mL molar concentrations are 0.3mol/L, the volume of potassium nitrate solution are poured into electrolyte tank 12 Account for the 60% of the volume of electrolyte tank 12.
The potassium nitrate solution that 250mL molar concentrations are 0.3mol/L, the volume of potassium nitrate solution are poured into the first salt room tank 6 The 100% of the volume of the first salt room 6 is accounted for, when electrodialytic membranes stack device is powered and produced, while using peristaltic pump 14 from deionized water Holding vessel 13 is passed through a certain amount of deionized water into the first salt room tank 6, it is ensured that potassium nitrate constant concentration exists in the first salt room tank 6 0.1-3mol/L。
The ammonium nitrate solution and ammonium nitrate crystals of 400mL saturation molar concentrations are poured into the second salt room surge tank 9, to keep Ammonium nitrate solution is saturated solution, and the second salt room surge tank 9 reaches overflow situation, while the second salt room tank 8 pours into 250mL saturations The ammonium nitrate solution of concentration, liquor capacity accounts for the 50% of the volume of the second salt room tank 8.
The ammonium chloride solution that 250mL molar concentrations are 1mol/L is poured into the 3rd salt room tank 7, the volume of ammonium chloride solution is accounted for The 100% of the volume of 3rd salt room tank 7, when electrodialytic membranes stack device is powered and produced, while using peristaltic pump 15 from deionized water Holding vessel 13 is passed through a certain amount of deionized water into the 3rd salt room tank 7, it is ensured that in the 3rd salt room tank 7 ammonium chloride concentration it is constant 0.1-6.5mol/L。
The Klorvess Liquid and potassium chloride of 400mL saturation molar concentrations, the 4th are poured into the 4th salt room surge tank 11 Salt room surge tank 11 reaches overflow situation, while the 4th salt room tank 10 pours into the Klorvess Liquid of 250mL saturated concentrations, solution body Product accounts for the 50% of the volume of the 4th salt room tank 10.
Open electrolyte immersible pump 23, the first salt room immersible pump 19, the second salt room immersible pump 21, the 3rd salt room immersible pump 20th, the 4th salt room immersible pump 22, makes electrolyte tank 12, the first salt room tank 6, the second salt room surge tank 9, the second salt room tank the 8, the 3rd The solution circulation flow that salt room tank 7, the 4th salt room tank are buffered in the 11, the 4th salt room tank 10 is dynamic with the bubble in remover；Wait to follow Circulation, which is moved, to be opened in dc source operation electrodialytic membranes stack device, the present embodiment after 10min using constant current operation, setting electric current Size is 3.00A.
The present embodiment tests electrodialytic membranes stack device voltage, test result such as Fig. 3 institutes during potassium nitrate is prepared Show, Fig. 3 is the electrodialytic membranes stack device voltage versus time curve figure of 1~embodiment of the embodiment of the present invention 3.
The present embodiment experiment terminate after determine the potassium ion of solution (target product) in the first salt room tank 6, nitrate ion, The concentration of chlorion, ammonium ion, calculates in product the mass fraction of potassium nitrate and changes into the mass fraction and energy of potassium oxide Consume (kwh/kg KNO3), determine and result of calculation as shown in table 1, table 1 be the product of 1~embodiment of embodiment 3 in potassium from Son, nitrate ion, chlorion, ammonium ion concentration and the potassium nitrate mass fraction of calculating and the quality for changing into potassium oxide Fraction and energy consumption (kwh/kg KNO3)。
Embodiment 2
Potassium nitrate is prepared using the preparation system shown in embodiment 1, comprised the following steps：
The potassium nitrate solution that 400mL molar concentrations are 0.3mol/L, the volume of potassium nitrate solution are poured into electrolyte tank 12 Account for the 60% of the volume of electrolyte tank 12.
The potassium nitrate solution that 250mL molar concentrations are 0.3mol/L, the volume of potassium nitrate solution are poured into the first salt room tank 6 The 100% of the volume of the first salt room 6 is accounted for, when electrodialytic membranes stack device is powered and produced, while using peristaltic pump 14 from deionized water Holding vessel 13 is passed through a certain amount of deionized water into the first salt room tank 6, it is ensured that potassium nitrate constant concentration exists in the first salt room tank 6 0.1-3mol/L。
The ammonium nitrate solution and ammonium nitrate crystals of 400mL saturation molar concentrations are poured into the second salt room surge tank 9, to keep Ammonium nitrate solution is saturated solution, and the second salt room surge tank 9 reaches overflow situation, while the second salt room tank 8 pours into 250mL saturations The ammonium nitrate solution of concentration, liquor capacity accounts for the 50% of the volume of the second salt room tank 8.
The ammonium chloride solution that 250mL molar concentrations are 1mol/L is poured into the 3rd salt room tank 7, the volume of ammonium chloride solution is accounted for The 100% of the volume of 3rd salt room tank 7, when electrodialytic membranes stack device is powered and produced, while using peristaltic pump 15 from deionized water Holding vessel 13 is passed through a certain amount of deionized water into the 3rd salt room tank 7, it is ensured that in the 3rd salt room tank 7 ammonium chloride concentration it is constant 0.1-6.5mol/L。
The Klorvess Liquid and potassium chloride of 400mL saturation molar concentrations, the 4th are poured into the 4th salt room surge tank 11 Salt room surge tank 11 reaches overflow situation, while the 4th salt room tank 10 pours into the Klorvess Liquid of 250mL saturated concentrations, solution body Product accounts for the 50% of the volume of the 4th salt room tank 10.
Open electrolyte immersible pump 23, the first salt room immersible pump 19, the second salt room immersible pump 21, the 3rd salt room immersible pump 20th, the 4th salt room immersible pump 22, makes electrolyte tank 12, the first salt room tank 6, the second salt room surge tank 9, the second salt room tank the 8, the 3rd The solution circulation flow that salt room tank 7, the 4th salt room tank are buffered in the 11, the 4th salt room tank 10 is dynamic with the bubble in remover；Wait to follow Circulation, which is moved, to be opened in dc source operation electrodialytic membranes stack device, the present embodiment after 10min using constant current operation, setting electric current Size is 4.00A.
The present embodiment tests electrodialytic membranes stack device voltage, test result such as Fig. 3 institutes during potassium nitrate is prepared Show, Fig. 3 is the electrodialytic membranes stack device voltage versus time curve figure of 1~embodiment of the embodiment of the present invention 3.
The present embodiment experiment terminate after determine the potassium ion of solution (target product) in the first salt room tank 6, nitrate ion, The concentration of chlorion, ammonium ion, calculates in product the mass fraction of potassium nitrate and changes into the mass fraction and energy of potassium oxide Consume (kwh/kg KNO3), determine and result of calculation as shown in table 1, table 1 be the product of 1~embodiment of embodiment 3 in potassium from Son, nitrate ion, chlorion, ammonium ion concentration and the potassium nitrate mass fraction of calculating and the quality for changing into potassium oxide Fraction and energy consumption (kwh/kg KNO3)。
Embodiment 3
Potassium nitrate is prepared using the preparation system shown in embodiment 1, comprised the following steps：
The potassium nitrate solution that 400mL molar concentrations are 1mol/L is poured into electrolyte tank 12, the volume of potassium nitrate solution is accounted for The 60% of the volume of electrolyte tank 12.
The potassium nitrate solution that 250mL molar concentrations are 1mol/L is poured into the first salt room tank 6, the volume of potassium nitrate solution is accounted for The 100% of the volume of first salt room 6, when electrodialytic membranes stack device is powered and produced, while being stored up using peristaltic pump 14 from deionized water Deposit tank 13 and be passed through a certain amount of deionized water into the first salt room tank 6, it is ensured that potassium nitrate constant concentration exists in the first salt room tank 6 0.1-3mol/L。
The sodium nitrate solution and nitric acid sodium crystal of 400mL saturation molar concentrations are poured into the second salt room surge tank 9, to keep Sodium nitrate solution is saturated solution, and the second salt room surge tank 9 reaches overflow situation, while the second salt room tank 8 pours into 250mL saturations The sodium nitrate solution of concentration, liquor capacity accounts for the 50% of the volume of the second salt room tank 8.
The sodium chloride solution that 250mL molar concentrations are 2mol/L is poured into the 3rd salt room tank 7, the volume of sodium chloride solution is accounted for The 100% of the volume of 3rd salt room tank 7, when electrodialytic membranes stack device is powered and produced, while using peristaltic pump 15 from deionized water Water store tank 13 is passed through a certain amount of deionized water into the 3rd salt room tank 7, it is ensured that sodium chloride concentration is constant in the 3rd salt room tank 7 In 0.1-6mol/L.
Klorvess Liquid and potassium chloride that 400mL saturation molar concentrations are are poured into the 4th salt room surge tank 11, the Four salt room surge tanks 11 reach overflow situation, while the 4th salt room tank 10 pours into the Klorvess Liquid of 250mL saturated concentrations, solution Volume accounts for the 50% of the volume of the 4th salt room tank 10.
Open electrolyte immersible pump 23, the first salt room immersible pump 19, the second salt room immersible pump 21, the 3rd salt room immersible pump 20th, the 4th salt room immersible pump 22 makes electrolyte tank 12, the first salt room tank 6, the second salt room surge tank 9, the second salt room tank the 8, the 3rd The solution circulation flow that salt room tank 7, the 4th salt room tank are buffered in the 11, the 4th salt room tank 10 is dynamic with the bubble in remover；Wait to follow Circulation, which is moved, to be opened in dc source operation electrodialytic membranes stack device, the present embodiment after 10min using constant current operation, setting electric current Size is 3.00A.
The present embodiment tests electrodialytic membranes stack device voltage, test result such as Fig. 3 institutes during potassium nitrate is prepared Show, Fig. 3 is the electrodialytic membranes stack device voltage versus time curve figure of 1~embodiment of the embodiment of the present invention 3.
The present embodiment experiment terminate after determine the potassium ion of solution (target product) in the first salt room tank 6, nitrate ion, The concentration of chlorion, sodium ion, calculates in product the mass fraction of potassium nitrate and changes into the mass fraction and energy consumption of potassium oxide (kw·h/kg KNO3), determine and result of calculation as shown in table 1, table 1 be the product of 1~embodiment of embodiment 3 in potassium ion, Nitrate ion, chlorion, Na ion concentration and the potassium nitrate of calculating mass fraction and change into potassium oxide mass fraction and Energy consumption (kwh/kg KNO3)。
Table 1
The explanation of above example is only intended to the method and its core concept for helping to understand the present invention.It should be pointed out that pair For one of ordinary skill in the art, under the premise without departing from the principles of the invention, the present invention can also be carried out some Improve and modify, these are improved and modification is also fallen into the protection domain of the claims in the present invention.To the disclosed embodiments Described above, enables the special technical staff in this area to realize or using the present invention, to a variety of modifications of these embodiments to ability It will be apparent for the professional and technical personnel of domain.Generic principles defined herein can not depart from the essence of the present invention In the case of refreshing or scope, realize in other embodiments.Therefore, the present invention is not intended to be limited to these realities shown in this article Example is applied, and is to fit to the most wide scope consistent with novel features with principles disclosed herein.

Claims (7)

1. a kind of preparation system of potassium nitrate, including：
Electrodialysis membrane stack, positive electrode, negative electrode, electrolyte sampling device, the first salting liquid generating means, the second salting liquid sample introduction Device, three-salt solution generating means, the 4th salting liquid sampling device, the first salting liquid storage device, the storage of the second salting liquid Device, three-salt solution storage device, the 4th salting liquid storage device, water storage apparatus and dc source；
The negative electrode is connected with the negative pole of the dc source；The positive electrode is connected with the positive pole of the dc source；Institute State negative electrode and the positive electrode is respectively arranged at the both sides of the electrodialysis membrane stack；
The electrodialysis membrane stack is internally formed cathode chamber, anode chamber, the first salt room, the second salt room, the 3rd salt room and the 4th salt room Six compartments；
The outlet of the electrolyte sampling device is connected with the charging aperture of the anode chamber, the discharging opening of the anode chamber with it is described The charging aperture of cathode chamber is connected, and the import of the electrolyte sampling device is connected with the discharging opening of the cathode chamber, constitutes electrolysis The circulation loop of liquid；
The outlet of the first salting liquid generating means is connected with the charging aperture of the first salt room, the first salting liquid generation The import of device is connected with the discharging opening of the first salt room, constitutes the circulation loop of the first salting liquid；
The outlet of the second salting liquid sampling device is connected with the charging aperture of the second salt room, the discharging of the second salt room Mouth is connected with the import of the second salting liquid storage device, the outlet of the second salting liquid storage device and second salt The import of solution sampling device is connected, and constitutes the circulation loop of the second salting liquid；
The outlet of the three-salt solution generating means is connected with the charging aperture of the 3rd salt room, the three-salt solution generation The import of device is connected with the discharging opening of the 3rd salt room, constitutes the circulation loop of three-salt solution；
The outlet of the 4th salting liquid sampling device is connected with the charging aperture of the 4th salt room, the discharging of the 4th salt room Mouth is connected with the import of the 4th salting liquid storage device, outlet and the 4th salt of the 4th salting liquid storage device The import of solution sampling device is connected, and constitutes the circulation loop of the 4th salting liquid；
The import of the outlet of the water storage apparatus respectively with the first salting liquid generating means, three-salt solution generating means It is connected；
The import of the first salting liquid storage device is connected with the outlet of the first salting liquid generating means by overflow manner；Institute The import for stating three-salt solution storage device is connected with the outlet of three-salt solution generating means by overflow manner.
2. preparation system according to claim 1, it is characterised in that：The electrodialysis membrane stack by cation-exchange membrane, every Alternate intervals are arranged to make up successively for net and anion-exchange membrane, and close to positive electrode and negative electrode are cation-exchange membrane, Anode chamber is formed between positive electrode and adjacent cation-exchange membrane, forms cloudy between negative electrode and adjacent cation-exchange membrane Pole room；The cation-exchange membrane and anion-exchange membrane arranged between anode chamber and cathode chamber by alternate intervals successively constitutes one Individual or multiple first salt rooms, the second salt room, the repeat unit of the 3rd salt room and the 4th salt room.
3. preparation system according to claim 1 or 2, it is characterised in that：The preparation system also includes clamping device, institute Stating clamping device is used to fix the negative electrode, positive electrode and electrodialysis membrane stack.
4. preparation system according to claim 1 or 2, it is characterised in that：Inside the electrodialysis membrane stack the first salt room and Ion exchange is realized between second salt room by interval of anion-exchange membrane, is handed between the second salt room and the 3rd salt room with cation Change film and realize ion exchange for interval, realize that ion is handed between the 3rd salt room and the 4th salt room by interval of anion-exchange membrane Change；Between 4th salt room and the first salt room of next repeat unit adjacent thereto ion is realized by interval of cation-exchange membrane Exchange.
5. a kind of preparation method of the potassium nitrate of preparation system described in any one in utilization Claims 1 to 44, its feature exists In comprising the following steps：
Strong electrolytic solution is transported in electrodialysis membrane stack anode chamber and cathode chamber by electrolyte sampling device；
Potassium nitrate solution is transported in the first salt of electrodialysis membrane stack room by the first salting liquid generating means, while water is stored Water in device is continually transported to certain flow in the first salting liquid generating means so that the first salting liquid generating means In the first salting liquid overflow in the first salting liquid storage device；
Nitrate solution is transported in the second salt of electrodialysis membrane stack room by the second salting liquid sampling device；
Chlorination salting liquid is transported in the salt room of electrodialysis membrane stack the 3rd by three-salt solution generating means, while water is stored Water in device is continually transported in three-salt solution generating means with certain flow so that three-salt solution generating means In three-salt solution overflow in three-salt solution storage device；
Klorvess Liquid is transported in the salt room of electrodialysis membrane stack the 4th by the 4th salting liquid sampling device.
The nitrate ion for opening nitrate solution in dc source, the second salt room passes through anion-exchange membrane under electric field action Move in the first salt room, the potassium ion of Klorvess Liquid is migrated under electric field action by cation-exchange membrane in the 4th salt room Into the first salt room, now potassium ion combines in the first salt room with nitrate ion and obtains potassium nitrate.
6. preparation method according to claim 5, it is characterised in that：It is molten that the strong electrolytic solution is selected from potassium hydroxide One or more in liquid, sodium nitrate solution, potassium nitrate solution and ammonium nitrate solution；It is molten that the chlorination salting liquid is selected from ammonium chloride One or more in liquid, sodium chloride solution and magnesium chloride solution；It is molten that the nitrate solution is selected from ammonium nitrate solution, sodium nitrate One or more in liquid and magnesium nitrate solution.
7. preparation method according to claim 5, it is characterised in that：
The strong electrolytic solution concentration is 0.01~2mol/L；
It is 0.01~3mol/L to make nitrate solution concentration in the first salt room generating means；Make nitre in the second salting liquid sampling device The molar concentration of acid salt solution is saturation molar concentration；Make in the 3rd salt room generating means chlorination concentration of salt solution be 0.01~ 6.5mol/L；The molar concentration for making Klorvess Liquid in the 4th salting liquid sampling device is saturation molar concentration.
CN201710376982.8A 2017-05-25 2017-05-25 The preparation system and preparation method of a kind of potassium nitrate Pending CN107162023A (en)

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CN109231377A (en) * 2018-08-28 2019-01-18 浙江工业大学 A kind of displacement electrodialysis methods preparing potassium fluoride by potassium chloride and ammonium fluoride
CN109534369A (en) * 2018-12-07 2019-03-29 杭州水处理技术研究开发中心有限公司 A kind of film is integrated to prepare lithium chloride device and method thereof
CN109569301A (en) * 2018-12-27 2019-04-05 山东天维膜技术有限公司 A method of producing potassium nitrate co-production acid
CN110318066A (en) * 2019-06-20 2019-10-11 青岛鼎海电化学科技有限公司 A kind of preparation method of tetra-alkyl ammonium hydroxide
CN112062218A (en) * 2020-09-02 2020-12-11 合肥工业大学 Device for continuously treating acid/alkali waste liquid and treatment method thereof
CN112218704A (en) * 2018-05-29 2021-01-12 迈姆布林有限股份公司 Method for producing lithium compounds by electrodialysis and device for carrying out said method

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CN103882468A (en) * 2014-03-28 2014-06-25 中国科学技术大学 Electrolysis-bipolar membrane electrodialysis system and method for producing lithium hydrate with lithium carbonate
CN105177619A (en) * 2015-07-28 2015-12-23 合肥工业大学 Device and method for preparing potassium sulphate
CN106362593A (en) * 2016-11-10 2017-02-01 合肥工业大学 Preparation system and preparation method of potassium sulfate

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Publication number Priority date Publication date Assignee Title
CN112218704A (en) * 2018-05-29 2021-01-12 迈姆布林有限股份公司 Method for producing lithium compounds by electrodialysis and device for carrying out said method
CN109231377A (en) * 2018-08-28 2019-01-18 浙江工业大学 A kind of displacement electrodialysis methods preparing potassium fluoride by potassium chloride and ammonium fluoride
CN109534369A (en) * 2018-12-07 2019-03-29 杭州水处理技术研究开发中心有限公司 A kind of film is integrated to prepare lithium chloride device and method thereof
CN109569301A (en) * 2018-12-27 2019-04-05 山东天维膜技术有限公司 A method of producing potassium nitrate co-production acid
CN110318066A (en) * 2019-06-20 2019-10-11 青岛鼎海电化学科技有限公司 A kind of preparation method of tetra-alkyl ammonium hydroxide
CN112062218A (en) * 2020-09-02 2020-12-11 合肥工业大学 Device for continuously treating acid/alkali waste liquid and treatment method thereof

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Application publication date: 20170915