CN111204779A - Fused salt production method for co-producing high-purity magnesium hydroxide, magnesium carbonate and nitrogen-potassium fertilizer - Google Patents
Fused salt production method for co-producing high-purity magnesium hydroxide, magnesium carbonate and nitrogen-potassium fertilizer Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
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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
- C01D9/10—Preparation by double decomposition with ammonium nitrate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
- C01F5/20—Magnesium hydroxide by precipitation from solutions of magnesium salts with ammonia
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/24—Magnesium carbonates
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/80—Compositional purity
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Abstract
A fused salt production method for coproducing high-purity magnesium hydroxide, magnesium carbonate and a nitrogen-potassium fertilizer relates to the technical field of chemical product production. The invention has the beneficial effects that: the invention adopts a co-production process which is complementary with the process for producing the magnesium hydroxide, utilizes the existing resources to obtain the maximum yield with the maximum efficiency, reduces the waste of raw materials, improves the added value of commodities, and has high utilization rate of process raw materials, high product purity and considerable economic benefit.
Description
Technical Field
The invention relates to the technical field of chemical product production, in particular to a fused salt production method for co-producing high-purity magnesium hydroxide, magnesium carbonate and nitrogen-potassium fertilizer.
Background
The by-products of molten salt grade potassium nitrate production at home and abroad are basically magnesium chloride and ammonium chloride. The production process is simple, chloride ions in the product can not be eradicated, and the obtained magnesium hydroxide product has low purity, so that the added value of the product is low. A co-production process matched with a process for producing high-end magnesium hydroxide by using a byproduct of molten salt-grade potassium nitrate production and high-purity magnesium carbonate is urgently needed. The production scheme proposed by the domestic patent (patent No. CN 109721082A) is similar to the present patent, but lacks scientific basis, for example, the patent proposes that solid magnesium oxide is reacted with 96% concentrated nitric acid to produce magnesium nitrate product, and the reaction is unreasonable by filtering, the concentrated nitric acid is reacted with the solid magnesium oxide, because the reaction is violent and the temperature is too high, on one hand, the reaction product is basically solid, so the filtration is not existed, on the other hand, the temperature exceeds the decomposition temperature of the nitric acid, and a large amount of nitrogen oxide toxic and harmful gas is produced in the reaction process. In addition, the method only comprises the step of magnesium precipitation, namely the step of generating magnesium hydroxide precipitate through the reaction with ammonia water, only 80-90% of magnesium ions can be removed generally due to the interference effect of ammonium ions, the purity of the molten salt grade potassium nitrate is required to be more than 99.8%, the content of the magnesium ions is required to be less than 0.001%, the content of chloride ions is required to be less than 0.01%, only 80-90% of the magnesium ions are removed, and the purity and the content of the magnesium ions of potassium nitrate produced in the subsequent steps are difficult to meet the specified requirements.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a process method for producing molten salt potassium nitrate and co-producing high-purity magnesium hydroxide, high-purity magnesium carbonate and a byproduct nitrogen-potassium fertilizer thereof.
The invention provides a molten salt production method for co-producing high-purity magnesium hydroxide, magnesium carbonate and nitrogen-potassium fertilizer, which comprises the following steps:
step 1, reacting magnesium slag or magnesia powder after lithium extraction in a salt lake with dilute nitric acid with the concentration of 40-60%, controlling the reaction temperature in a mode of diluting and cooling by using magnesium hydroxide washing water or magnesium carbonate washing water to obtain magnesium nitrate neutralizing liquid, adding an auxiliary agent to remove heavy metals, and filtering to obtain refined magnesium nitrate solution; the addition amount of the auxiliary agent is determined according to the content of impurities in the neutralizing solution; the auxiliary agent is NB-727 auxiliary agent.
Step 2, adding the refined magnesium nitrate solution and prepared 25-30% ammonia water or gas ammonia into a high-speed stirring reaction kettle, heating to 90 ℃, adding 0.1-3% of crystal form regulator for reaction, and filtering after the reaction is finished to obtain a magnesium hydroxide crude product with the particle size of 0.5-2 microns and an ammonium nitrate mother liquor A; the crystal form regulator is a citrate compound; the reaction formula of the step is as follows:
Mg(NO3)2+2NH3+2H20=Mg(OH)2↓+2NH4NO3
in the reaction, as the concentration of ammonium ions is higher and higher along with the reaction, magnesium ions cannot be completely precipitated into magnesium hydroxide due to reversibility of the reaction under interference between the ions, the precipitation rate of the magnesium ions is usually about 90%, the quality of potassium nitrate products is influenced due to incomplete precipitation of the magnesium ions in the mother liquor A, and the residual magnesium salts remained in the mother liquor need to enter the step 3 for continuous reaction;
and 3, adding residual magnesium nitrate precipitated by ammonium bicarbonate into the ammonium nitrate mother liquor A obtained in the step 2, wherein the mass ratio of the magnesium nitrate to the ammonium bicarbonate is as follows in terms of ammonium carbonate: 1:1.05-1.08, performing reaction at the temperature of 50-80 ℃, performing reaction for 1.5-2.5h, pumping the solid-liquid product after the reaction into an aging pot by using a pump for aging for 7-9h, filtering and separating to obtain a magnesium carbonate product and a low-calcium magnesium ammonium nitrate mother liquor B, washing the obtained magnesium carbonate with clean water for 2 times to obtain a high-purity magnesium carbonate product, sending the washing water to the step 1 to serve as dilution water, and allowing the ammonium nitrate mother liquor B to enter the next step to produce potassium nitrate; the reaction formula of the step is as follows:
5Mg(NO3)2+5(NH4)2CO3+5H2O=4MgCO3·Mg(OH)2·4H2O↓+10NH4NO3+CO2↑
step 4, adjusting the pH value of the ammonium nitrate mother liquor B obtained in the step 3 to 6-7 by using dilute nitric acid to react with the processed potassium chloride, reacting by using the waste heat of the mother liquor, cooling to 5-30 ℃ after the reaction is finished, separating to obtain a crude potassium nitrate product and a mother liquor C, recrystallizing and refining the crude potassium nitrate to obtain a molten salt-grade potassium nitrate product, and combining the recrystallized mother liquor into a reaction kettle of ammonium nitrate and potassium chloride; the reaction formula of the step is as follows:
NH4NO3+KCl=KNO3(Low temperature crystallization) + NH4Cl
Step 5, concentrating the mother liquor C generated in the step 4, cooling to 60 ℃, separating to obtain a binary nitrogen-potassium fertilizer, drying, packaging and warehousing, and sending the separated mother liquor D to a reaction pot of ammonium nitrate and potassium chloride;
and 6, washing the obtained magnesium hydroxide crude product with clear water for 2 times, sending the washing water to the step 1 as dilution water, drying and crushing to obtain a high-purity magnesium hydroxide product.
In the step 1, the reaction temperature is controlled to be less than 83 ℃, and the concentration of nitric acid in the reaction liquid is controlled to be less than 30% in the reaction process.
In the step 2, the ammonia water is excessive by 5-10% according to the reaction equilibrium proportion.
In the step 4, potassium chloride is added in an excess of 1-5% according to the reaction equilibrium proportion.
The invention has the beneficial effects that: the invention adopts the co-production process which is matched with the high-purity magnesium carbonate and is used for producing the high-end magnesium hydroxide by the byproduct of the molten salt level potassium nitrate production, and the co-production process is complementary with the magnesium hydroxide production process, so that the existing resources are utilized to the maximum degree to obtain the maximum yield, the waste of the raw materials is reduced, the commodity added value is improved, the utilization rate of the raw materials of the process is high, the product purity is high, and the economic benefit is considerable;
in the step 3, the residual magnesium ions in the ammonium nitrate liquid after the magnesium hydroxide is filtered react with ammonium carbonate under the action of the aid to perform precipitation reaction to generate basic magnesium carbonate, and the magnesium ions are further removed after the step of precipitating the magnesium hydroxide, so that the magnesium precipitation rate is higher, and the quality of a fused salt product is ensured; by using the organic additive as a medium crystal agent, the crystal form of the magnesium hydroxide directionally grows to obtain a high-quality magnesium hydroxide product and a high-purity magnesium carbonate product, and meanwhile, all the additives are fully recycled under specific conditions, so that the production cost of the molten salt is reduced to a great extent, and a promotion effect is brought to future solar energy storage in China.
Drawings
FIG. 1 is a schematic view of the process of the present invention.
Detailed Description
Example 1, step 1, reacting magnesium slag after lithium extraction from a salt lake with dilute nitric acid with the concentration of 40-60%, controlling the reaction temperature below 83 ℃ in a magnesium hydroxide washing water or magnesium carbonate washing water dilution cooling mode to obtain magnesium nitrate neutralized liquid, adding an auxiliary agent to remove heavy metals, and filtering to obtain refined magnesium nitrate solution 1573.6Kg with the mass concentration of 47%;
step 2, adding 606Kg of 30% prepared ammonia water (with 7% excess) and refined magnesium nitrate solution into a high-speed stirring reaction kettle, heating to 90 ℃, adding 0.1% crystal form regulator for reaction, filtering after the reaction is finished to obtain 275.6Kg of magnesium hydroxide crude product with the particle size of 0.5-2 microns and ammonium nitrate mother liquor A, and detecting the concentration of residual magnesium ions in the solution to know that the magnesium ion conversion rate in the step is 85%;
and 3, adding residual magnesium nitrate precipitated by ammonium bicarbonate into the ammonium nitrate mother liquor A obtained in the step 2, wherein the mass ratio of the magnesium nitrate to the ammonium bicarbonate is as follows in terms of ammonium carbonate: 1:1.07, carrying out reaction at the temperature of 50-80 ℃, carrying out reaction for 1.5h, pumping a solid-liquid product after the reaction into an aging pot by using a pump for aging for 7h, filtering and separating to obtain a magnesium carbonate product and a low-calcium magnesium ammonium nitrate mother liquor B, washing the obtained magnesium carbonate with clear water for 2 times to obtain 68.9Kg of a high-purity magnesium carbonate product with the purity of 99.4 percent and the contents of chloride ions and iron ions of less than 0.01 percent, sending the washing water to the step 1 as dilution water, and sending the ammonium nitrate mother liquor B to the next step for producing potassium nitrate; the total magnesium deposition rate of the step 2 and the step 3 is 99.7 percent;
and 4, adjusting the pH value of the ammonium nitrate mother liquor B obtained in the step 3 to 6-7 by using dilute nitric acid, reacting with 805.2Kg (excess of 8%) of processed potassium chloride, reacting by using the waste heat of the mother liquor, cooling to 30 ℃ after the reaction is finished, separating to obtain 1020.4Kg of crude potassium nitrate product and mother liquor C, recrystallizing and refining the crude potassium nitrate product to obtain 997.8Kg of molten salt-grade potassium nitrate product with the purity of 99.96%, the content of magnesium ions of 0.0006% and the content of chloride ions of 0.005%, and combining the recrystallized mother liquor into a reaction kettle of ammonium nitrate and potassium chloride.
And 5, concentrating the mother liquor C generated in the step 4, cooling to 60 ℃, separating to obtain 622.3Kg of binary nitrogen potassium fertilizer, drying, packaging and warehousing, and sending the separated mother liquor D to a reaction pot of ammonium nitrate and potassium chloride.
And 6, washing the obtained high-end magnesium hydroxide crude product with clean water for 2 times, sending the washing water to the step 1 as diluting water, drying and crushing to obtain 250.3Kg of high-purity magnesium hydroxide product with the purity of 99.6 percent and the whiteness of 95.5 percent.
Example 2, step 1, reacting magnesium slag after lithium extraction from a salt lake with dilute nitric acid with the concentration of 40-60%, controlling the reaction temperature below 83 ℃ in a magnesium hydroxide washing water or magnesium carbonate washing water dilution cooling mode to obtain magnesium nitrate neutralized liquid, adding an auxiliary agent to remove heavy metals, and filtering to obtain refined magnesium nitrate solution 3287.2Kg with the concentration of 45%;
step 2, adding prepared 1247Kg (10% excess) of 30% ammonia water and refined magnesium nitrate solution into a high-speed stirring reaction kettle, heating to 90 ℃, adding 2% of crystal form regulator for reaction, filtering after the reaction is finished to obtain 550.9Kg of magnesium hydroxide crude product with the particle size of 0.5-2 microns and ammonium nitrate mother liquor A, and detecting the concentration of residual magnesium ions in the solution to find that the magnesium ion conversion rate in the step is 89%;
and 3, adding residual magnesium nitrate precipitated by ammonium bicarbonate into the ammonium nitrate mother liquor A obtained in the step 2, wherein the mass ratio of the magnesium nitrate to the ammonium bicarbonate is as follows in terms of ammonium carbonate: 1:1.08, the reaction temperature is between 50 and 80 ℃, the reaction time is 2 hours, the solid-liquid product after the reaction is finished is pumped into an aging pot by a pump to be aged for 8 hours, a magnesium carbonate product and a low-calcium magnesium ammonium nitrate mother liquor B are obtained by filtration and separation, the obtained magnesium carbonate is washed by clean water for 2 times to obtain 92.7Kg of high-purity magnesium carbonate product with the purity of 99.5 percent and the content of chloride ions and iron ions of less than 0.01 percent, the washing water is sent to the step 1 to be used as dilution water, the ammonium nitrate mother liquor B enters the next step to produce potassium nitrate, and the total magnesium deposition rate of the step 2 and the step 3 is 99.94 percent
And 4, adjusting the pH value of the ammonium nitrate mother liquor B obtained in the step 3 to 6-7 by using dilute nitric acid, reacting with 1580.6Kg (excess 5%) of processed potassium chloride, reacting by using the waste heat of the mother liquor, cooling to 20 ℃ after the reaction is finished, separating to obtain 2341.9Kg of crude potassium nitrate product and mother liquor C, recrystallizing and refining the crude potassium nitrate product to obtain 1960Kg of molten salt-grade potassium nitrate product with the purity of 99.98%, the content of magnesium ions of 0.0004% and the content of chloride ions of 0.002%, and combining the recrystallized mother liquor into a reaction kettle of ammonium nitrate and potassium chloride.
And 5, concentrating the mother liquor C generated in the step 4, cooling to 60 ℃, separating to obtain 1278.7Kg of binary nitrogen potassium fertilizer, drying, packaging and warehousing, and sending the separated mother liquor D to a reaction pot of ammonium nitrate and potassium chloride.
And 6, washing the obtained high-end magnesium hydroxide crude product with clean water for 2 times, sending the washing water to the step 1 as diluting water, drying and crushing to obtain 510.3Kg of high-purity magnesium hydroxide product with the purity of 99.4 percent and the whiteness of 95 percent.
Example 3, step 1, reacting the bitter earth powder with dilute nitric acid with a concentration of 40-60%, diluting with magnesium hydroxide washing water or magnesium carbonate washing water to reduce the temperature to below 83 ℃ to obtain magnesium nitrate neutralized solution, adding an auxiliary agent to remove heavy metals, and filtering to obtain refined magnesium nitrate solution 3081.7Kg with a concentration of 48%;
step 2, adding 1430Kg (5% excess) of prepared 25% ammonia water and refined magnesium nitrate solution into a high-speed stirring reaction kettle, heating to 90 ℃, adding 3% of crystal form regulator for reaction, filtering after the reaction is finished to obtain 537.2Kg of magnesium hydroxide crude product with the particle size of 0.5-2 microns and ammonium nitrate mother liquor A, and detecting the concentration of residual magnesium ions in the solution to know that the magnesium ion conversion rate in the step is 87%;
and 3, adding residual magnesium nitrate precipitated by ammonium bicarbonate into the ammonium nitrate mother liquor A obtained in the step 2, wherein the mass ratio of the magnesium nitrate to the ammonium bicarbonate is as follows in terms of ammonium carbonate: 1:1.05, performing reaction at the temperature of 50-80 ℃, performing reaction for 2.5 hours, pumping a solid-liquid product after the reaction into an aging pot by using a pump, aging for 9 hours, filtering and separating to obtain a magnesium carbonate product and a low-calcium magnesium ammonium nitrate mother liquor B, washing the obtained magnesium carbonate with clear water for 2 times to obtain 116.7Kg of high-purity magnesium carbonate product with the purity of 99.3 percent and the contents of chloride ions and iron ions of less than 0.01 percent, sending the washing water to the step 1 as dilution water, and allowing the ammonium nitrate mother liquor B to enter the next step for producing potassium nitrate, wherein the total magnesium deposition rate of the step 2 and the step 3 is 99.5 percent;
and 4, adjusting the pH value of the ammonium nitrate mother liquor B obtained in the step 3 to 6-7 by using dilute nitric acid, reacting with 1640.3Kg (excess 10%) of processed potassium chloride, reacting by using the waste heat of the mother liquor, cooling to 5 ℃ after the reaction is finished, separating to obtain 2545.1Kg of crude potassium nitrate product and mother liquor C, recrystallizing and refining the crude potassium nitrate product to obtain 2015Kg of molten salt-grade potassium nitrate product with the purity of 99.90%, the content of magnesium ions of 0.0008% and the content of chloride ions of 0.007%, and combining the recrystallized mother liquor into a reaction kettle of ammonium nitrate and potassium chloride.
And 5, concentrating the mother liquor C generated in the step 4, cooling to 60 ℃, separating to obtain 1369.5Kg of binary nitrogen potassium fertilizer, drying, packaging and warehousing, and sending the separated mother liquor D to a reaction pot of ammonium nitrate and potassium chloride.
And 6, washing the obtained high-end magnesium hydroxide crude product with clean water for 2 times, sending the washing water to the step 1 as diluting water, drying and crushing to obtain 506.8Kg of high-purity magnesium oxide product with the purity of 99.7 percent and the whiteness of 96 percent.
Claims (4)
1. A fused salt production method for co-producing high-purity magnesium hydroxide, magnesium carbonate and nitrogen-potassium fertilizer is characterized by comprising the following steps: the method comprises the following steps:
step 1, reacting magnesium slag or magnesia powder after lithium extraction in a salt lake with dilute nitric acid with the concentration of 40-60%, controlling the reaction temperature in a mode of diluting and cooling by using magnesium hydroxide washing water or magnesium carbonate washing water to obtain magnesium nitrate neutralizing liquid, adding an auxiliary agent to remove heavy metals, and filtering to obtain refined magnesium nitrate solution;
step 2, adding the refined magnesium nitrate solution and prepared excessive 25-30% ammonia water into a high-speed stirring reaction kettle, heating to 90 ℃, adding 0.1-3% of crystal form regulator for reaction, and filtering after the reaction is finished to obtain a magnesium hydroxide crude product with the particle size of 0.5-2 microns and an ammonium nitrate mother liquor A;
and 3, adding residual magnesium nitrate precipitated by ammonium bicarbonate into the ammonium nitrate mother liquor A obtained in the step 2, wherein the mass ratio of the magnesium nitrate to the ammonium bicarbonate is as follows in terms of ammonium carbonate: 1:1.05-1.08, performing reaction at the temperature of 50-80 ℃, performing reaction for 1.5-2.5h, pumping the solid-liquid product after the reaction into an aging pot by using a pump for aging for 7-9h, filtering and separating to obtain a magnesium carbonate product and a low-calcium magnesium ammonium nitrate mother liquor B, washing the obtained magnesium carbonate with clean water for 2 times to obtain a high-purity magnesium carbonate product, sending the washing water to the step 1 to serve as dilution water, and allowing the ammonium nitrate mother liquor B to enter the next step to produce potassium nitrate;
step 4, adjusting the pH value of the ammonium nitrate mother liquor B obtained in the step 3 to 6-7 by using dilute nitric acid to react with the processed potassium chloride, reacting by using the waste heat of the mother liquor, cooling to 5-30 ℃ after the reaction is finished, separating to obtain a crude potassium nitrate product and a mother liquor C, recrystallizing and refining the crude potassium nitrate to obtain a molten salt-grade potassium nitrate product, and combining the recrystallized mother liquor into a reaction kettle of ammonium nitrate and potassium chloride;
step 5, concentrating the mother liquor C generated in the step 4, cooling to 60 ℃, separating to obtain a binary nitrogen-potassium fertilizer, drying, packaging and warehousing, and sending the separated mother liquor D to a reaction pot of ammonium nitrate and potassium chloride;
and 6, washing the obtained magnesium hydroxide crude product with clear water for 2 times, sending the washing water to the step 1 as dilution water, drying and crushing to obtain a high-purity magnesium hydroxide product.
2. The molten salt production method for co-producing high-purity magnesium hydroxide, magnesium carbonate and nitrogen-potassium fertilizer according to claim 1, which is characterized in that: in the step 1, the reaction temperature is controlled to be less than 83 ℃, and the concentration of nitric acid in the reaction liquid is controlled to be less than 30% in the reaction process.
3. The molten salt production method for co-producing high-purity magnesium hydroxide, magnesium carbonate and nitrogen-potassium fertilizer according to claim 1, which is characterized in that: in the step 2, the ammonia water is excessive by 5-10% according to the reaction equilibrium proportion.
4. The molten salt production method for co-producing high-purity magnesium hydroxide, magnesium carbonate and nitrogen-potassium fertilizer according to claim 1, which is characterized in that: in the step 4, 5-10% of potassium chloride is added according to the reaction equilibrium proportion.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114956134A (en) * | 2022-06-28 | 2022-08-30 | 安徽胜达化工科技有限公司 | Co-production process of high-purity magnesium hydroxide and nitrogen potassium fertilizer |
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Application publication date: 20200529 |