CN109956486A - Potassium nitrate purification system and method - Google Patents
Potassium nitrate purification system and method Download PDFInfo
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- CN109956486A CN109956486A CN201711341442.2A CN201711341442A CN109956486A CN 109956486 A CN109956486 A CN 109956486A CN 201711341442 A CN201711341442 A CN 201711341442A CN 109956486 A CN109956486 A CN 109956486A
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- Prior art keywords
- potassium nitrate
- filter cake
- filtrate
- washing
- purification
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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
- C01D9/16—Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
A kind of method of purification of potassium nitrate, includes the following steps: S1: after raw material is sufficiently washed, being separated by solid-liquid separation, obtains filter cake and filtrate；S2: it dissolves the filter cake and forms saturated solution, then KOH solution is added in the saturated solution and sufficiently reacts, after the sediment after filtering out reaction, solution is recrystallized, finally washing, drying crystallization.Potassium nitrate of the invention proposes that method simple production process, the potassium nitrate product purity produced reach 99.99% or more, meet high-purity grade of potassium nitrate standard (industrial potassium nitrate GB1918-2011), meets the potassium nitrate product requirement of optical glass.In particular, the method for purification of potassium nitrate of the invention can use agricultural grade potassium nitrate, technical grade potassium nitrate and strengthen optical glass salt bath inactivation potassium nitrate as raw material, production cost is reduced.
Description
Technical field
The present invention relates to potassium nitrate purification technique fields, more particularly to one kind with agricultural grade potassium nitrate, technical grade nitric acid
Potassium or optical glass salt bath inactivation potassium nitrate are the method for feedstock purification potassium nitrate.
Background technique
With the continuous development of information industry and opto-electronics, demand of the international market to optical glass increasingly rises,
Increase high-purity grade of potassium nitrate demand year by year.The intensity of simple glass reduces with thickness and is substantially reduced, and is not able to satisfy electronics
The requirement of display touch screen technology development exchanges work by low-temperature ion for the demand for adapting to social progress and development in science and technology
Skill the chemical strengthening of ordinary flat thin glass is improved glass machinery performance seem especially it is necessary to.
Industrialization continuous production show ion exchange quality by quality, different processing parameters of potassium nitrate etc. because
The influence of element, these factors influence KNO3Salt bath activity reduces the phenomenon that even final complete deactivation.KNO3The active reduction of salt bath
The quality of product (optical glass), KNO will be directly affected3As the ion exchange source of chemically enhancing glass, activity to from
Sub- exchange process plays conclusive influence.(1) raw material KNO3Purity, technical grade KNO3Mainly contain impurity Na+、Ca2+、Mg2+、
Ba2+、Cl-Plasma.According to production practices, KNO used in chemically reinforced glass3Raw material, in KNO3Ca in fused salt2+、Sr2+、Ba2+Deng
Foreign ion will be to K after running up to a certain concentration+—Na+Exchange generates ameliorating effect and depression effect.(2) high temperature KNO3Point
Solution, document are recorded, KNO3337~339 DEG C of fusing point, it can be decomposed in 400 DEG C of environment and release oxygen and generate KNO2, continue to add
Heat will generate K2O.In ion exchange process, KNO3Fused salt is placed in hot environment for a long time, and decomposed generation will certainly occur
KNO2Even K2O, the NO on the one hand generated2 -It will constantly be accumulated in fused salt, and inhibit ion-exchange reactions activity；On the other hand,
Decompose the O generated2And other gases will be adsorbed in the surface of glass, hinder K+With Na+Exchange.(3) ion exchange is dirty
Dye, simple glass contain the oxides such as a considerable amount of CaO, NaO and MgO, and in ion exchange process, glass and fused salt slot are in height
It is impregnated for a long time in thermohaline bath and Na is precipitated+、Ca2+、Mg2+Equal foreign ions, cause KNO3Active reduce of fused salt is even lost completely
It is living, finally influence product quality.
The enterprise of the optical glass of China's production at present, in KNO3The potassium nitrate raw material more renewed is shut down after salt bath inactivation, is made
KNO after inactivation3It is not recycled.Domestic optical glass is in based on import potassium nitrate with potassium nitrate market length, and into
High-purity grade of 18000~20000 yuan/ton of potassium nitrate market price of mouth, it is high-purity grade about 11000~12000 yuan/ton of potassium nitrate domestic.
The problem of present invention mainly solves two aspects, is on the one hand directed to KNO3Deactivation cause finds out the potassium nitrate warp shut down and cleaned out
Processing makes the new method brought back to life again, improves the recycling rate of waterused of raw material, saves production cost；On the other hand, the present invention uses
High-purity grade of potassium nitrate of agricultural grade potassium nitrate or technical grade Production of Potassium Nitrate solves China and relies on high-purity grade of nitre of high price import for a long time
Sour potassium problem.
Summary of the invention
To solve drawbacks described above, the present invention provides a kind of preparation method of potassium nitrate, includes the following steps: S1: by raw material
Sufficiently after washing, separation of solid and liquid obtains filter cake and filtrate；S2: it dissolves the filter cake and forms saturated solution, then add KOH solution
Enter and sufficiently reacted in the saturated solution, after the sediment after filtering out reaction, solution is recrystallized, separation of solid and liquid is filtered
Cake and filtrate are finally washed, the dry filter cake.
According to an embodiment of the present invention, the raw material is agricultural grade potassium nitrate, technical grade potassium nitrate or reinforcing optics
Glass salt bath inactivates potassium nitrate.
The raw material is crushed to 8- before washing in the S1 step by another embodiment according to the present invention
50 mesh.
KOH solution is added in the S2 step under the conditions of 95~110 DEG C in another embodiment according to the present invention, adjusts
Save pH to 9~11.
Another embodiment according to the present invention, washing is repeatedly washing in the S2 step, wherein after primary washing
Filtrate afterwards is used for previous washing.
Another embodiment according to the present invention, further includes: S3: the filtrate in S1 step is heated up and is evaporated, after evaporation
Mother liquor carry out crystallisation by cooling, obtain slurry, be separated by solid-liquid separation, obtain filter cake and filtrate；The filter cake is back to S1 step
Suddenly it is used as raw material.
Another embodiment according to the present invention, further includes: S4: the filtrate spent ion exchange resin in S2 step is removed
Metal ion is back to washing of the S1 step for raw material after HNO3 solution adjustment pH value to neutrality is then added.
The present invention also provides a kind of purification systems of potassium nitrate, comprising: preceding washing unit is used for washing material, and carries out
Separation of solid and liquid forms filter cake and filtrate；Chemical subtraction unit, the filter for separating KOH solution and the preceding washing unit
The saturated solution of cake reacts, and recrystallizes after filtering out sediment to solution, and separation of solid and liquid obtains filter cake and filtrate；It is washed after and
Unit is washed, the filter cake separated for washing the chemical subtraction unit；Wherein solidliquid mixture object in the purification system
Material relies on gravity from flowing in the system.
According to an embodiment of the present invention, the nitric acid purification system, further includes: evaporative crystallization unit, for steaming
The filtrate sending out preceding washing unit described and separating forms crystallization.
Another embodiment according to the present invention, the nitric acid purification system, further includes: physics impurity removed system, with from
Sub-exchange resin removes the metal ion in the filtrate that the chemical subtraction unit is separated, and the adjustment of HNO3 solution is then added
The preceding washing unit is returned it to after pH value to neutrality.
Potassium nitrate of the invention proposes that method simple production process, the potassium nitrate product purity produced reach
99.99% or more, meet high-purity grade of potassium nitrate standard (industrial potassium nitrate GB1918-2011), meets the nitric acid of optical glass
Potassium product requirement.In particular, the method for purification of potassium nitrate of the invention can use agricultural grade potassium nitrate, technical grade potassium nitrate with
And strengthening optical glass salt bath inactivation potassium nitrate is raw material, reduces production cost.The present invention moves towards arrangement by material, facilitates life
Produce operation；Material enters next equipment using potential energy gravity flow, reduces intermediate conveying process, saves power consumption, shortens slurry pipe
Road conveying distance overcomes the problems such as line clogging, abrasion, noise；The present invention produces to obtain Na in product+Content≤100ppm,
Ca2+、Mg2+Total amount≤1ppm.KNO3Mother liquid evaporation, the present invention carry out triple effect evaporation, condensing hot air furnace using novel heat-conducting material
It utilizes, saves water resource and save power consumption simultaneously.
Detailed description of the invention
Fig. 1 is the process flow diagram of potassium nitrate method of purification of the invention.
Fig. 2 is the schematic diagram of potassium nitrate purification system of the invention.
Wherein, the reference numerals are as follows:
1- crushing plant；2- raw material washing tank；3a, 3b, 3c, 3d, 3e- separation equipment；4- chemical subtraction equipment；5a,5b-
Filter plant；6-KNO3Recrystallize equipment；7- once washing equipment；8- secondary washing equipment；9- drying equipment；10- physics removes
Miscellaneous equipment；11- evaporation equipment；12- crystallizer.
Specific embodiment
It elaborates With reference to embodiment to the present invention.
Embodiment 1
As depicted in figs. 1 and 2, a certain number of reinforcing optical glass salt bath inactivation potassium nitrate (Na are taken first+Content 3500
~5500ppm) with crushing plant 1 it is crushed to 20 mesh.
Breakdown products are sent to preceding washing unit, preceding washing system includes raw material washing tank 2 and separation equipment 3a.It is broken to produce
Object enters washing tank 2, is washed 0.5 hour with deionized water in room temperature, subsequently into separation equipment 3a solid-liquid under normal temperature conditions
Separation, obtains filter cake and filtrate.
The filter cake that separation equipment 3a is separated enters chemical subtraction unit, and chemical subtraction system includes chemical subtraction equipment
4, filter plant 5a, KNO3Recrystallize equipment 6 and separation equipment 3b.Under the conditions of 100 DEG C of heating and thermal insulations, filter cake is removed in chemistry
Saturation dissolution is formed in miscellaneous equipment 4.Under 100 DEG C of heat-retaining conditions, KOH solution is added in chemical subtraction equipment 4, pH is adjusted to
10, Ca (OH) is filtered by filter plant 5a2、Mg(OH)2Precipitating finally obtains qualified saturation lysate (Ca2++Mg2+≤
10ppm).Solution is introduced into KNO3It recrystallizes equipment 6 and carries out 5 grades of crystallisation by cooling, temperature is down to 25 DEG C by 100 DEG C, is crystallized
Slurry obtains filter cake and filtrate after separation equipment 3b separation of solid and liquid.
Washing unit after the filter cake that separation equipment 3b is separated is sent into, rear washing unit include once washing equipment 7,
Separation equipment 3c, 3d and secondary washing equipment 8.Filter cake is sufficiently washed in once washing equipment 7, and wash time 0.5 is small
Shi Hou is separated by solid-liquid separation in separation equipment 3c, obtains filter cake and filtrate.Filtrate is back to chemical subtraction equipment 4 for shape
At saturated solution.Filter cake enters in secondary washing equipment 8, and it is small to carry out secondary washing wash time 0.5 to filter cake with deionized water
Shi Hou is separated by solid-liquid separation in separation equipment 3d, obtains filter cake and filtrate.Filtrate returns in once washing equipment 7 for washing
Wash filter cake.The present embodiment is not intended to limit the present invention, those skilled in the art can according to need really for washing twice
The fixed number specifically washed, Na in filter cake after control washing+Content≤100ppm.The filter cake separated from separation equipment 3d
It is dried into drying unit, obtains high-purity grade of potassium nitrate, potassium nitrate purity is 99.99%.
The filtrate separated from separation equipment 3b enters physics impurity removed system, and physics impurity removed system includes filter plant 5b
With physics impurity removing equipment 10.The filtrate that separation equipment 3b is separated is maintained at 25 DEG C of temperature, after filter plant 5b filtering,
Ca is further removed into 10 spent ion exchange resin of physics impurity removing equipment2+、Mg2+Then HNO is added in ion3Solution is by pH value
Neutrality is recalled to, Ca is obtained2++Mg2+The KNO of≤20ppb3It is saturated clear liquid.The saturation stillness of night is back to the washing for raw material of raw material washing tank 2
It washs.
The filtrate separated from separation equipment 3a enters evaporation element, and evaporation element includes that evaporation equipment 11, crystallization are set
Standby 12 and separation equipment 3e.The filtrate separated from separation equipment 3a is sent into evaporation equipment 11, evaporates at 100 DEG C.Then
5 grades of crystallisation by cooling are carried out to the mother liquor after evaporation in crystallizer 12, temperature is down to 25 DEG C by 100 DEG C, obtains slurry,
It is separated through separation equipment 3e, obtains filter cake and filtrate, filter cake is sent to raw material sink 2.
Filtrate in evaporation equipment 11 continues to evaporate at 100 DEG C.Mother liquor after evaporation carries out 5 grades of crystallisation by cooling, temperature
25 DEG C are down to by 100 DEG C, obtains slurry, is separated by solid-liquid separation, filter cake and filtrate are obtained, filter cake is handled by mixed salt, and filtrate is used
It sizes mixing in mixed salt vapo(u)rization system.
It is 45% that slurry, which need to add adjusting slurry to adjust solid content (mass content), in the present embodiment, before being separated by solid-liquid separation every time, is adjusted
Slurries are the filtrate that each separation equipment itself is separated.Recycling condensed water in evaporation process, for the washing of raw material and molten
Solution.
Each equipment is rationally arranged in the present embodiment, so that the flowing of solid-liquid mixed slurry enters dependent on gravitional force gravity flow
Next equipment.Therefore, it is possible to reduce intermediate conveying process saves power consumption, shortens slurry piping feeding distance, overcomes pipeline
The problems such as blocking, abrasion, noise.Simultaneously as solid-liquid mixed slurry is flowed dependent on gravitional force, i.e., need to stand between equipment
Body setting, to save the space occupied of system, provides the utilization rate of workshop.
Embodiment 2
Other than it will strengthen optical glass salt bath inactivation potassium nitrate and be changed to technical grade potassium nitrate, other steps and embodiment 1
It is identical.
Obtained potassium nitrate purity is 99.99%.
Certainly, the present invention can also have other various embodiments, without deviating from the spirit and substance of the present invention, ripe
It knows those skilled in the art and makes various corresponding changes and modifications, but these corresponding changes and change in accordance with the present invention
Shape all should fall within the scope of protection of the appended claims of the present invention.
Claims (10)
1. a kind of method of purification of potassium nitrate, which comprises the steps of:
S1: after raw material is sufficiently washed, separation of solid and liquid obtains filter cake and filtrate；
S2: it dissolves the filter cake and forms saturated solution, then KOH solution is added in the saturated solution and sufficiently reacts, filters out
After sediment after reaction, solution is recrystallized, separation of solid and liquid obtains filter cake and filtrate, finally washs, the dry filter
Cake.
2. the method for purification of potassium nitrate according to claim 1, which is characterized in that the raw material be agricultural grade potassium nitrate,
Technical grade potassium nitrate strengthens optical glass salt bath inactivation potassium nitrate.
3. the method for purification of potassium nitrate according to claim 2, which is characterized in that in the S1 step, in washing
It is preceding that the raw material is crushed to 8-50 mesh.
4. the method for purification of potassium nitrate according to claim 1, which is characterized in that at 95~110 DEG C in the S2 step
Under the conditions of, KOH solution is added, adjusts pH to 9~11.
5. the method for purification of potassium nitrate according to claim 1, which is characterized in that washing is repeatedly to wash in the S2 step
It washs, wherein the filtrate after rear primary washing is used for previous washing.
6. the method for purification of potassium nitrate according to claim 1, which is characterized in that further include:
S3: the filtrate in S1 step being heated up and is evaporated, and the mother liquor after evaporation is carried out crystallisation by cooling, obtains slurry, through solid
Liquid separation, obtains filter cake and filtrate；The filter cake is back to S1 step as raw material.
7. the method for purification of potassium nitrate according to claim 1, which is characterized in that further include:
S4: the filtrate spent ion exchange resin in S2 step is removed into metal ion, HNO is then added3Solution adjusts pH value into
Property after, be back to S1 step for raw material washing.
8. a kind of purification system of potassium nitrate characterized by comprising
Preceding washing unit is used for washing material, and be separated by solid-liquid separation and form filter cake and filtrate；
The saturated solution of chemical subtraction unit, the filter cake for separating KOH solution and the preceding washing unit reacts, and filters
Solution is recrystallized after sediment out, separation of solid and liquid obtains filter cake and filtrate；And
Washing unit afterwards, the filter cake separated for washing the chemical subtraction unit；
Wherein solidliquid mixture material relies on gravity from flowing in the system in the purification system.
9. nitric acid purification system according to claim 8, which is characterized in that further include:
Evaporative crystallization unit forms crystallization for evaporating the filtrate that the preceding washing unit is separated.
10. nitric acid purification system according to claim 8, which is characterized in that further include:
Physics impurity removed system, spent ion exchange resin remove the metal in the filtrate that the chemical subtraction unit is separated from
Then HNO is added in son3The preceding washing unit is returned it to after solution adjustment pH value to neutrality.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201711341442.2A CN109956486A (en) | 2017-12-14 | 2017-12-14 | Potassium nitrate purification system and method |
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| CN201711341442.2A CN109956486A (en) | 2017-12-14 | 2017-12-14 | Potassium nitrate purification system and method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110482574A (en) * | 2019-08-21 | 2019-11-22 | 四川金山制药有限公司 | Photoelectricity grade potassium nitrate purifying technique |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105236452A (en) * | 2015-11-06 | 2016-01-13 | 化工部长沙设计研究院 | Technology for producing highly pure potassium nitrate through reaction of sodium nitrate and potassium chloride |
-
2017
- 2017-12-14 CN CN201711341442.2A patent/CN109956486A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105236452A (en) * | 2015-11-06 | 2016-01-13 | 化工部长沙设计研究院 | Technology for producing highly pure potassium nitrate through reaction of sodium nitrate and potassium chloride |
Non-Patent Citations (2)
| Title |
|---|
| 朱韶红: "《学生学习内容疑难问题解析 初中化学》", 31 May 2012, 东北师范大学出版社 * |
| 魏成广等: "《中国钾盐工业概览》", 31 July 2009, 上海交通大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110482574A (en) * | 2019-08-21 | 2019-11-22 | 四川金山制药有限公司 | Photoelectricity grade potassium nitrate purifying technique |
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