CN105439175A - Method for directly producing potassium nitrate - Google Patents
Method for directly producing potassium nitrate Download PDFInfo
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- CN105439175A CN105439175A CN201511007756.XA CN201511007756A CN105439175A CN 105439175 A CN105439175 A CN 105439175A CN 201511007756 A CN201511007756 A CN 201511007756A CN 105439175 A CN105439175 A CN 105439175A
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- saltpetre
- water
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- potassium
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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
- C01D9/04—Preparation with liquid nitric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/03—Preparation from chlorides
- C01B7/035—Preparation of hydrogen chloride from chlorides
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for directly producing potassium nitrate. The method comprises the following steps: (1) adding potassium chloride and nitric acid into water, stirring for reaction, carrying out cooling and crystallization, and then carrying out solid-liquid separation to obtain a potassium nitrate product I and a mother liquid I; (2) conducting further cooling and crystallization on the mother liquid I, and then carrying out solid-liquid separation to obtain a crude potassium nitrate product and a mother liquid II; (3) re-dissolving the crude potassium nitrate product in water, and carrying out re-crystallization and solid-liquid separation to obtain a potassium nitrate product II; (4) allowing the mother liquid II and water to flow through a diffusion dialyzer at the same time, so as to obtain a hydrochloric acid solution containing a little nitric acid and a recovery liquid containing potassium ions; replacing the water in step (1) with the recovery liquid for the next round of potassium nitrate preparation, so as to recycle the recovery liquid. The method is low in production cost; the potassium chloride conversion ratio and the one-time finished product ratio are high, and a potassium nitrate product with high purity and stable quality can be obtained; not only are acids recovered, but also potassium is recycled, so that the potassium loss is reduced, and the comprehensive utilization ratio of resources is increased.
Description
Technical field
The present invention relates to the method for producing saltpetre.
Background technology
Saltpetre is a kind of important inorganic chemical product, industrial saltpetre and agricultural saltpetre is mainly divided into according to purposes, current Production of Potassium Nitrate method mainly with Repone K and nitrate for feedstock conversion is produced, its typical method mainly contains double decomposition, ion exchange method, extraction process etc.
The technology of preparing potassium nitrate by means of double decomposition, be mainly raw material with Repone K and magnesium nitrate or ammonium nitrate, deficiency is wherein: saltpetre solubleness in the magnesium chloride and ammonium chloride of by-product is comparatively large, not only reduces the quality of by-product product, also causes the potassium ion rate of recovery low; Recycling Mother Solution amount is large, and steam output is also larger, causes product cost higher.
The technology of saltpetre produced by extraction agent, mainly with Repone K, nitric acid organic solvent for raw material, its weak point is: the extraction agent selected is organic solvent, to the toxic effect of human body, solid surface can adsorb a certain amount of solvent, causes solvent loss, increases production cost; From system, isolated solvent is not only containing nitric acid, and containing hydrochloric acid, causes separation process complicated.
Ion exchange method produces the technology of saltpetre, mainly with ammonium nitrate and Repone K for raw material, its weak point is: utilize ion exchange resin for exchange carrier, by upper potassium with wash the production that potassium process completes saltpetre and ammonium chloride.There is saltpetre concentration in generative process low, evaporation cost is high; Equipment requirements is high, increases the problems such as production cost, has explosivity simultaneously, there is higher potential safety hazard high.
Summary of the invention
The present invention is directed to that prior art cost is high, equipment is complicated, technical process is long, product quality is low, energy consumption is high, pollute the problems such as large, provide a kind of direct method to produce the method for saltpetre.
Direct method provided by the invention produces the method for saltpetre, comprises the following steps:
(1) Repone K and nitric acid are added to the water and carry out stirring reaction, react complete and carry out cooling saltpetre is fully separated out, then carry out solid-liquid separation, gained solids is product saltpetre, and gained liquid is mother liquor I;
(2) cooling mother liquor I makes crystallisate separate out further further, and then carry out solid-liquid separation, gained solids is crude product saltpetre, and gained liquid is mother liquor II;
(3) by heavy for crude product saltpetre soluble in water, then carry out recrystallization and saltpetre is fully separated out, recrystallization is complete carries out solid-liquid separation, and gained solids is product saltpetre;
(4) mother liquor II and water are flowed through after diffusion dialysis device carries out diffusion dialysis simultaneously, obtain the hydrochloric acid soln containing a small amount of nitric acid and the Ethylene recov containing potassium ion; Ethylene recov replaces the water in step (1) to be used for the preparation of lower whorl nitroxylic acid potassium, to recycle Ethylene recov.
The mol ratio of described Repone K, nitric acid and water is 1: 1-1.4: 7-9.
The temperature of the stirring reaction in described step (1) is 50-90 DEG C.
Crystallisation by cooling in described step (1) carries out under the temperature condition of 20-40 DEG C.
Crystallisation by cooling in described step (2) carries out under the temperature condition of-7 to 0 DEG C.
In described step (3), the mass ratio of crude product saltpetre and water is 0.4-2.4: 1.
In described step (4), the flow of the water and mother liquor II that flow through diffusion dialysis device is respectively 10-80L/min and 10-60L/min.
Described diffusion dialysis device is made up of 2-8 group flat diffusion dialysis device serial or parallel connection; Often organize flat device to be made up of 15-30 flat dialysis unit.
The exchange membrane of described diffusion dialysis device is anion-exchange membrane, and described anion-exchange membrane is aromatic polyether class composite membrane.
Compared with prior art, the present invention has the following advantages:
1, wide raw material source, cheap, production cost significantly reduces;
2, equipment is simple, and technical process is few, and production process energy consumption is low;
3, the separation method of the present invention's employing is simple to operation, easily separated, reduces washing Finished product processThe, effectively reduce Recycling Mother Solution amount, reduce the consumption of raw materials for production in production process;
4, Repone K transformation efficiency is high, and disposable yield rate is high, can obtain the high and stay-in-grade potassium nitrate product of purity;
5, the present invention adopts two-step crystallization, namely ensure that quality product turn improves production efficiency;
Not only 6, the present invention utilizes diffusion dialysis device water to be become hydrochloric acid soln containing a small amount of nitric acid, and mother liquor II becomes the Ethylene recov containing potassium ion, has reclaimed acid but also has achieved the recycle of potassium, reduced the loss of potassium, improve comprehensive resource utilization rate.
Embodiment
Embodiment 1
(1) Repone K, nitric acid and water are joined in retort, stirring reaction 1 hour under the temperature condition of 50-63 DEG C, react complete and reaction solution is sent into cooling crystallizer, under the temperature condition of 20-26 DEG C, make saltpetre sufficient crystallising separate out, then solid-liquid separation is carried out by whizzer, the solids of solid-liquid separation gained is product saltpetre, and the liquid of gained is mother liquor I; The mol ratio of described Repone K, nitric acid and water is 1: 1: 7;
(2) mother liquor I is sent into freezing and crystallizing device, make saltpetre sufficient crystallising separate out, then carry out solid-liquid separation by whizzer under the temperature condition of-7 to-5 DEG C, the solids of solid-liquid separation gained is crude product saltpetre, and gained liquid is mother liquor II;
(3) be the proportion relation of 0.45: 1 by the mass ratio of crude product saltpetre and water, under temperature 30 DEG C of conditions, by heavy for crude product saltpetre soluble in water, then sending into cooling crystallizer makes saltpetre sufficient crystallising separate out, crystallization is complete carries out solid-liquid separation by whizzer, and the solids carrying out solid-liquid separation gained is product saltpetre;
(4) flow controlling water and mother liquor II is respectively 10L/min and 10L/min, makes mother liquor II and current carry out diffusion dialysis through diffusion dialysis device, obtains the hydrochloric acid soln containing a small amount of nitric acid and the Ethylene recov containing potassium ion; Ethylene recov replaces the water in step (1) to be used for the preparation of lower whorl nitroxylic acid potassium, is recycled to make Ethylene recov.
Embodiment 2
(1) Repone K, nitric acid and water are joined in retort, stirring reaction 1.2 hours under the temperature condition of 63-76 DEG C, react complete and reaction solution is sent into cooling crystallizer, under the temperature condition of 26-33 DEG C, make saltpetre sufficient crystallising separate out, then solid-liquid separation is carried out by whizzer, the solids of solid-liquid separation gained is product saltpetre, and the liquid of gained is mother liquor I; The mol ratio of described Repone K, nitric acid and water is 1: 1.2: 8;
(2) mother liquor I is sent into freezing and crystallizing device, make saltpetre sufficient crystallising separate out, then carry out solid-liquid separation by whizzer under the temperature condition of-5 to-3 DEG C, the solids of solid-liquid separation gained is crude product saltpetre, and gained liquid is mother liquor II;
(3) be the proportion relation of 1: 1 by the mass ratio of crude product saltpetre and water, under temperature 60 C condition, by heavy for crude product saltpetre soluble in water, then sending into cooling crystallizer makes saltpetre sufficient crystallising separate out, crystallization is complete carries out solid-liquid separation by whizzer, and the solids carrying out solid-liquid separation gained is product saltpetre;
(4) flow controlling water and mother liquor II is respectively 80L/min and 60L/min, makes mother liquor II and current carry out diffusion dialysis through diffusion dialysis device, obtains the hydrochloric acid soln containing a small amount of nitric acid and the Ethylene recov containing potassium ion; Ethylene recov replaces the water in step (1) to be used for the preparation of lower whorl nitroxylic acid potassium, is recycled to make Ethylene recov.
Embodiment 3
(1) Repone K, nitric acid and water are joined in retort, stirring reaction 2 hours under the temperature condition of 76-90 DEG C, react complete and reaction solution is sent into cooling crystallizer, under the temperature condition of 33-40 DEG C, make saltpetre sufficient crystallising separate out, then solid-liquid separation is carried out by whizzer, the solids of solid-liquid separation gained is product saltpetre, and the liquid of gained is mother liquor I; The mol ratio of described Repone K, nitric acid and water is 1: 1.4: 9, and nitric acid adopts concentration to be the nitric acid of 60%.
(2) mother liquor I is sent into freezing and crystallizing device, make saltpetre sufficient crystallising separate out, then carry out solid-liquid separation by whizzer under the temperature condition of-3 to 0 DEG C, the solids of solid-liquid separation gained is crude product saltpetre, and gained liquid is mother liquor II;
(3) be the proportion relation of 2: 1 by the mass ratio of crude product saltpetre and water, under temperature 90 DEG C of conditions, by heavy for crude product saltpetre soluble in water, then sending into cooling crystallizer makes saltpetre sufficient crystallising separate out, crystallization is complete carries out solid-liquid separation by whizzer, and the solids carrying out solid-liquid separation gained is product saltpetre;
(4) flow controlling water and mother liquor II is respectively 45L/min and 35L/min, makes mother liquor II and current carry out diffusion dialysis through diffusion dialysis device, obtains the hydrochloric acid soln containing a small amount of nitric acid and the Ethylene recov containing potassium ion; Ethylene recov replaces the water in step (1) to be used for the preparation of lower whorl nitroxylic acid potassium, is recycled to make Ethylene recov.
Above-mentioned diffusion dialysis device is made up of 2-8 group flat diffusion dialysis device serial or parallel connection; Often organize flat device to be made up of 15-30 flat dialysis unit; Adopt anion-exchange membrane in return film, anion-exchange membrane adopts aromatic polyether class composite membrane.
The implication that in the present invention, Ethylene recov recycles is: the water used in step (1) just uses when first time prepares saltpetre, after obtaining mother liquor II through step (4), later preparation mother liquor II replaces water and Repone K, nitric acid to be prepared saltpetre.
Claims (9)
1. direct method produces a method for saltpetre, it is characterized in that comprising the following steps:
(1) Repone K and nitric acid are added to the water and carry out stirring reaction, react complete and carry out cooling saltpetre is fully separated out, then carry out solid-liquid separation, gained solids is product saltpetre, and gained liquid is mother liquor I;
(2) cooling mother liquor I makes crystallisate separate out further further, and then carry out solid-liquid separation, gained solids is crude product saltpetre, and gained liquid is mother liquor II;
(3) by heavy for crude product saltpetre soluble in water, then carry out recrystallization and saltpetre is fully separated out, recrystallization is complete carries out solid-liquid separation, and gained solids is product saltpetre;
(4) mother liquor II and water are flowed through after diffusion dialysis device carries out diffusion dialysis simultaneously, obtain the hydrochloric acid soln containing a small amount of nitric acid and the Ethylene recov containing potassium ion; Ethylene recov replaces the water in step (1) to be used for the preparation of lower whorl nitroxylic acid potassium, to recycle Ethylene recov.
2. direct method according to claim 1 produces the method for saltpetre, it is characterized in that: the mol ratio of described Repone K, nitric acid and water is 1: 1-1.4: 7-9.
3. the direct method according to claims 1 produces the method for saltpetre, it is characterized in that: the temperature of the stirring reaction in described step (1) is 50-90 DEG C.
4. the direct method according to claims 1 produces the method for saltpetre, it is characterized in that: the crystallisation by cooling in described step (1) carries out under the temperature condition of 20-40 DEG C.
5. the direct method according to claims 1 produces the method for saltpetre, it is characterized in that: the crystallisation by cooling in described step (2) carries out under the temperature condition of-7 to 0 DEG C.
6. direct method according to claim 1 produces the method for saltpetre, it is characterized in that: in described step (3), the mass ratio of crude product saltpetre and water is 0.4-2.4: 1, and the heavy molten temperature condition of crude product saltpetre is 30-90 DEG C.
7. direct method according to claim 1 produces the method for saltpetre, and it is characterized in that: in described step (4), the flow of the water and mother liquor II that flow through diffusion dialysis device is respectively 10-80L/min and 10-60L/min.
8. direct method according to claim 1 produces the method for saltpetre, it is characterized in that: described diffusion dialysis device is made up of 2-8 group flat diffusion dialysis device serial or parallel connection; Often organize flat device to be made up of 15-30 flat dialysis unit.
9. direct method according to claim 8 produces the method for saltpetre, and it is characterized in that: the exchange membrane of described diffusion dialysis device is anion-exchange membrane, described anion-exchange membrane is aromatic polyether class composite membrane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511007756.XA CN105439175A (en) | 2015-12-30 | 2015-12-30 | Method for directly producing potassium nitrate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511007756.XA CN105439175A (en) | 2015-12-30 | 2015-12-30 | Method for directly producing potassium nitrate |
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| CN105439175A true CN105439175A (en) | 2016-03-30 |
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| CN201511007756.XA Pending CN105439175A (en) | 2015-12-30 | 2015-12-30 | Method for directly producing potassium nitrate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107651698A (en) * | 2017-10-25 | 2018-02-02 | 安徽胜达化工科技有限公司 | A kind of production method of potassium nitrate crystals |
| CN108439435A (en) * | 2018-03-24 | 2018-08-24 | 山东天化学股份有限公司 | A kind of method that direct method prepares potassium nitrate |
| CN111410938A (en) * | 2020-01-21 | 2020-07-14 | 山西沃锦新材料股份有限公司 | Binary molten salt and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1064063A (en) * | 1992-02-27 | 1992-09-02 | 山东省昌乐县硝酸盐厂 | Utilize the method for rare nitric acid production saltpetre |
| CN101182014A (en) * | 2007-12-15 | 2008-05-21 | 文水县振兴化肥有限公司 | Preparation technique of potassium nitrate |
| CN104108730A (en) * | 2013-04-19 | 2014-10-22 | 刘玮 | Preparation process of potassium nitrate |
-
2015
- 2015-12-30 CN CN201511007756.XA patent/CN105439175A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1064063A (en) * | 1992-02-27 | 1992-09-02 | 山东省昌乐县硝酸盐厂 | Utilize the method for rare nitric acid production saltpetre |
| CN101182014A (en) * | 2007-12-15 | 2008-05-21 | 文水县振兴化肥有限公司 | Preparation technique of potassium nitrate |
| CN104108730A (en) * | 2013-04-19 | 2014-10-22 | 刘玮 | Preparation process of potassium nitrate |
Non-Patent Citations (2)
| Title |
|---|
| 徐铜文等: "《离子交换膜的制备与应用技术》", 30 September 2008, 化学工业出版社 * |
| 贾荣宝等: "《精细化工产品生产工艺精选》", 30 June 1998, 安徽科学技术出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107651698A (en) * | 2017-10-25 | 2018-02-02 | 安徽胜达化工科技有限公司 | A kind of production method of potassium nitrate crystals |
| CN108439435A (en) * | 2018-03-24 | 2018-08-24 | 山东天化学股份有限公司 | A kind of method that direct method prepares potassium nitrate |
| CN111410938A (en) * | 2020-01-21 | 2020-07-14 | 山西沃锦新材料股份有限公司 | Binary molten salt and preparation method thereof |
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Application publication date: 20160330 |