CN110255586A - The method that accurate control separation sodium nitrite, sodium chloride produce fused salt grade sodium nitrate - Google Patents
The method that accurate control separation sodium nitrite, sodium chloride produce fused salt grade sodium nitrate Download PDFInfo
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- CN110255586A CN110255586A CN201910522023.1A CN201910522023A CN110255586A CN 110255586 A CN110255586 A CN 110255586A CN 201910522023 A CN201910522023 A CN 201910522023A CN 110255586 A CN110255586 A CN 110255586A
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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
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
- C01B21/50—Nitrous acid; Salts thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
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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
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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
- 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
- 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
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Abstract
The invention discloses the methods that accurate control separation sodium nitrite, sodium chloride produce fused salt grade sodium nitrate, it is related to sodium nitrite, sodium nitrate technology for producing field, separation, the separation of chlorination magnesium addition including sodium nitrite, the separation of sodium chloride as impurity, recrystallization prepare the several steps of fused salt grade sodium nitrate, finally obtain sodium nitrite Grade A and fused salt grade sodium nitrate.The beneficial effects of the present invention are: use the neutralizer of nitric acid producing system vent gas treatment for raw material, it is at low cost, it eliminates pollution and obtains being worth higher product；Relative to previous method, this method separates sodium nitrite to neutralize in concentrate sodium nitrate concentration as judgment basis, and parameter value is accurate, rigorous, and it is excellent to obtain sodium nitrite product quality；Solution circulate operation sodium nitrate, each impurity is completely separated with product in solution, no wastage of material, and production cost is low；Gained sodium nitrate product purity is high of the invention, meets fused salt grade sodium nitrate product standard.
Description
Technical field
The present invention relates to sodium nitrite, sodium nitrate technology for producing field, it is specifically related to accurately control separation nitrous
The method that sour sodium, sodium chloride produce fused salt grade sodium nitrate.
Background technique
Domestic solar energy heat build-up power industry is risen in recent years, substitutes coal fired power generation, belongs to green energy resource, country props up energetically
It holds.The mixture that heat-storage medium is sodium nitrate and potassium nitrate is used in solar energy heat build-up, i.e. solar energy heat-storage fused salt, quality is wanted
Ask high, demand is big (million tons or more).There is the basis for producing agriculture potassium nitrate, industrial sodium nitrate in our company, therefore develops too
It is positive can heat accumulation fused salt condition it is good, develop solar energy heat-storage fused salt small investment on this basis, and can be country needed for meeting market
Green Development do one's bit.
The exhaust gas that our company is generated using sodium carbonate and production nitric acid at present carries out the production of sodium nitrate as raw material, now produces
Sodium nitrate is technical grade, and fused salt grade quality requirement is not achieved.And raw material soda ash (Na2CO3) and water body in impurity it is more.With raw material
Investment, wherein accumulated impurity will be more and more for mother liquor concentrations；Therefore impurity, which must be isolated, could improve sodium nitrate product quality.
The separation of sodium chloride as impurity in sodium nitrate, not existing data can inquire, right in previous sodium nitrate production
The separation for neutralizing sodium nitrite and sodium nitrate in concentrate is in the past reference with empirical value, separates sodium nitrite product qualification rate
It is low, no science, accurate parameter.
Summary of the invention
In order to overcome disadvantage of the existing technology, production technology is improved, the present invention proposes accurate control separation nitrous acid
The method that sodium, sodium chloride produce fused salt grade sodium nitrate solves the problems, such as that impurity separates in nitric acid process for producing sodium, provides science
Promoted sodium nitrate, sodium nitrite quality rigorous scheme, thus reduce production cost, reduce material waste.
The technical solution of the present invention is as follows: the method that accurate control separation sodium nitrite, sodium chloride produce fused salt grade sodium nitrate,
The following steps are included:
S01, the separation of sodium nitrite will be concentrated with the neutralizer of nitrogen oxides in soda ash, crystallize, nitrous acid is obtained by filtration
Sodium product and mother liquor A；Obtain main 98.5~99.5%(of the content butt of sodium nitrite product), reach industrial sodium nitrite first-class
Product and the above standard；
S02, the separation of chlorination magnesium addition, S01 obtain mother liquor A and nitric acid are added to convert, and remaining sodium nitrite is made all to generate nitric acid
Sodium, sodium nitrate solution liquid pass through 3-6 condensing crystallizing, it is isolated industry grade sodium nitrate and mother liquor B, mother liquor B in sodium chloride accumulate
Tiring out to the concentration of Cl- is 50-150g/L, and sodium chloride and sodium nitrate reach total saturation point under room temperature, and sodium nitrate is common with sodium chloride
It is precipitated, technical grade sodium nitrate product quality dissatisfaction can be made, which must be handled, and it is miscellaneous that mother liquor B contains sodium chloride, magnesium chloride
Matter is added the sodium carbonate with the amount of magnesium chloride same substance according to measurement, magnesium carbonate is settled out, through magnesium carbonate and filter is obtained by filtration
Liquid；Reaction principle: MgCl2+ Na2CO3= 2NaCl + MgCO3↓；
S02 is obtained filtrate and continues to be concentrated by S03, the separation of sodium chloride as impurity, so that liquor capacity is reduced 20~30%, chlorination
When sodium crystallization is precipitated, continue to heat concentrate to 100-120 DEG C, the density of solution is 1.3~1.5Kg/L, NO3-Concentration be
380~500g/L, Cl-Concentration be 70-110g/L when, be filtered, separating at high temperature sodium chloride, isolated hot mother liquor
C crystallisation by cooling obtains nitric acid sodium crystal and cold mother liquor D, and cold mother liquor D re-evaporation isolates sodium chloride, so circulation by sodium chloride with
Sodium nitrate distinguishes complete output；
S04, recrystallization prepare fused salt grade sodium nitrate, and the industrial sodium nitrate that S02, S03 are obtained is female through first time condensing crystallizing in S02
Liquid water washing removes the sodium chloride of part attachment, isolates crystal, then dissolved with steam condensate (SC), recrystallized, separated
To fused salt grade sodium nitrate and mother liquor E.
In the S01, the concentration be neutralizer is concentrated into sodium nitrate in solution concentration be 50~500g/L,
The crystallization be 10-60 DEG C at a temperature of carry out.
The concentration of nitric acid in the S02 is 40%.
In the S04, containing big in the cleaning solution obtained after first time condensing crystallizing mother liquor water washing in S02
Sodium nitrate and sodium chloride are measured, the concentration into the evaporation of sodium nitrate evaporator, control NO3- is 380~500g/L, and separating at high temperature goes out
Sodium chloride, the isolated industrial nitric acid sodium crystal of filtrate crystallisation by cooling finally also obtain fused salt into production system circular treatment
Grade sodium nitrate.
It is recycled in solution after the mother liquor E is added to S02 plus nitric acid conversion.
First time condensing crystallizing mother liquid coming in the S02, chloride content is low, and industrial sodium nitrate is washed with it can be with
The sodium chloride of part attachment is removed, while reducing the elution amount of sodium nitrate.
The steam condensate (SC) is the used steam of sodium nitrate mother liquor concentrations crystallization, passes through tubular heat exchanger with solution
Condensed water is formed after heat exchange.
The beneficial effects of the present invention are: the present invention uses the neutralizer fused salt grade nitre of nitric acid producing system vent gas treatment
Sour sodium, it is at low cost, it eliminates pollution and obtains being worth higher product；It is relatively previous with experience than recast state modulator
Method, this method separate sodium nitrite to neutralize in concentrate sodium nitrate concentration as judgment basis, and parameter value is accurate, tight
Sincerely, the sodium nitrite product quality obtained is excellent；Solution circulate operation, each impurity is completely separated with product in solution, nothing
Wastage of material, production cost are low；Gained sodium nitrate product purity is high of the invention, meets fused salt grade sodium nitrate product standard, product
For solar energy thermal-power-generating, energy conservation and environmental protection.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Embodiment 1, S01, the separation of sodium nitrite will be concentrated into 1000Kg soda ash with the neutralizer of nitrogen oxides
The concentration of sodium nitrate is 50g/L, under conditions of 10 DEG C of temperature, crystallizes, sodium nitrite product 210Kg and mother liquor A is obtained by filtration；?
To the main content 98.5(butt of sodium nitrite product), reach industrial sodium nitrite Grade A and the above standard；
S02, the separation of chlorination magnesium addition, S01 obtain mother liquor A and 172Kg nitric acid (concentration 40%) are added to convert, and make remaining nitrous acid
Sodium all generates sodium nitrate, and sodium nitrate solution liquid passes through 3-6 condensing crystallizing, when Chlorine in Solution sodium builds up to Cl-Concentration
For 50g/L, sodium chloride and sodium nitrate reach total saturation point under room temperature, are separated to industrial grade sodium nitrate 45Kg and mother liquor B；Mother liquor B
Containing sodium chloride, chlorination magnesium addition, 0.35Kg sodium carbonate is added according to measurement, magnesium carbonate is settled out, through magnesium carbonate is obtained by filtration
0.25Kg and filtrate；
S02 is obtained filtrate and continues concentrate solution volume reduction 30% by S03, and sodium chloride mass crystallization is precipitated, by concentrate
At 100 DEG C, the density of solution is 1.3Kg/L, NO3 -Concentration be 380g/L, Cl-Concentration be 70g/L when filter, it is Isolating chlorinated
Sodium 14Kg, isolated mother liquor crystallisation by cooling obtain nitric acid sodium crystal 54Kg；Cold mother liquor re-evaporation isolates sodium chloride, heat
Mother liquor crystallisation by cooling obtains sodium nitrate, and so circulation obtains sodium nitrate 96Kg.
S04, recrystallization prepare fused salt grade sodium nitrate, and the industrial sodium nitrate 195Kg that S02, S03 are obtained is through first time in S02
(cleaning solution enters the evaporation of sodium nitrate evaporator to condensing crystallizing mother liquor water washing, and sodium nitrate, recrystallization system are obtained after Isolating chlorinated sodium
Standby fused salt grade sodium nitrate), the sodium chloride of part attachment is removed, isolates crystal, then dissolved with steam condensate (SC), recrystallizes, divide
From obtaining fused salt grade sodium nitrate 144Kg, separation mother liquor enter S02's plus nitric acid conversion after solution in carry out condensing crystallizing
Circulation production.
Embodiment 2, S01, the separation of sodium nitrite will be concentrated into 2200Kg soda ash with the neutralizer of nitrogen oxides
The concentration of sodium nitrate is 300g/L, under conditions of 40 DEG C of temperature, crystallizes, sodium nitrite product 445Kg and mother liquor A is obtained by filtration；
Obtain the main content 99.1%(butt of sodium nitrite product), reach industrial sodium nitrite Grade A and the above standard；
S02, the separation of chlorination magnesium addition, S01 obtain mother liquor A and 387Kg nitric acid (concentration 40%) are added to convert, and make remaining nitrous acid
Sodium all generates sodium nitrate, and sodium nitrate solution liquid is separated to industrial grade sodium nitrate 99Kg and mother liquor B by 5 condensing crystallizings, molten
Accumulation of sodium chloride is to Cl in liquid-Concentration be 100g/L, sodium chloride and sodium nitrate reach total saturation point under room temperature；Mother liquor B contains
Sodium chloride, chlorination magnesium addition are added 0.8Kg sodium carbonate according to measurement, are settled out magnesium carbonate, magnesium carbonate 0.7Kg is obtained by filtration
And filtrate；
S02 is obtained filtrate and continues concentrate solution volume reduction 25% by S03, and sodium chloride mass crystallization is precipitated, by concentrate
At 110 DEG C, the density of solution is 1.4Kg/L, NO3 -Concentration be 440g/L, Cl-Concentration be 90g/L when filter, it is Isolating chlorinated
Sodium 30.2Kg, isolated mother liquor crystallisation by cooling obtain nitric acid sodium crystal 118Kg；Cold mother liquor re-evaporation isolates chlorination
Sodium, hot mother liquor crystallisation by cooling obtain sodium nitrate, and so circulation obtains sodium nitrate 219Kg.
S04, recrystallization prepare fused salt grade sodium nitrate, and the industrial sodium nitrate 436Kg that S02, S03 are obtained is through first time in S02
(cleaning solution enters the evaporation of sodium nitrate evaporator to condensing crystallizing mother liquor water washing, and sodium nitrate, recrystallization system are obtained after Isolating chlorinated sodium
Standby fused salt grade sodium nitrate), the sodium chloride of part attachment is removed, isolates crystal, then dissolved with steam condensate (SC), recrystallizes, divide
From obtaining fused salt grade sodium nitrate 326Kg, separation mother liquor enter S02's plus nitric acid conversion after solution in carry out condensing crystallizing
Circulation production.
Embodiment 3, S01, the separation of sodium nitrite will be concentrated into 3000Kg soda ash with the neutralizer of nitrogen oxides
The concentration of sodium nitrate is 500g/L, under conditions of temperature 60 C, crystallizes, sodium nitrite product 590Kg and mother liquor A is obtained by filtration；
Obtain the main content 99.5%(butt of sodium nitrite product), reach industrial sodium nitrite Grade A and the above standard；
S02, the separation of chlorination magnesium addition, S01 obtain mother liquor A and 541Kg nitric acid (concentration 40%) are added to convert, and make remaining nitrous acid
Sodium all generates sodium nitrate, and sodium nitrate solution liquid passes through 3-6 condensing crystallizing, when Chlorine in Solution sodium builds up to Cl-Concentration
For 150g/L, sodium chloride and sodium nitrate reach total saturation point under room temperature, are separated to industrial grade sodium nitrate 135Kg and mother liquor B；Mother liquor
B contains sodium chloride, chlorination magnesium addition, and 1.09Kg sodium carbonate is added according to measurement, magnesium carbonate is settled out, through magnesium carbonate is obtained by filtration
0.9Kg and filtrate；
S02 is obtained filtrate and continues concentrate solution volume reduction 20% by S03, and sodium chloride mass crystallization is precipitated, by concentrate
At 120 DEG C, the density of solution is 1.5Kg/L, NO3 -Concentration be 500g/L, Cl-Concentration be 110g/L when filter, separate chlorine
Change sodium 42.4Kg, isolated mother liquor crystallisation by cooling obtains nitric acid sodium crystal 163Kg；Cold mother liquor re-evaporation isolates chlorination
Sodium, hot mother liquor crystallisation by cooling obtain sodium nitrate, and so circulation obtains sodium nitrate 292Kg.
S04, recrystallization prepare fused salt grade sodium nitrate, and the industrial sodium nitrate 590Kg that S02, S03 are obtained is through first time in S02
(cleaning solution enters the evaporation of sodium nitrate evaporator to condensing crystallizing mother liquor water washing, and sodium nitrate, recrystallization system are obtained after Isolating chlorinated sodium
Standby fused salt grade sodium nitrate), the sodium chloride of part attachment is removed, isolates crystal, then dissolved with steam condensate (SC), recrystallizes, divide
From obtaining fused salt grade sodium nitrate 440Kg, separation mother liquor enter S02's plus nitric acid conversion after solution in carry out condensing crystallizing
Circulation production.
Claims (5)
1. the method that accurate control separation sodium nitrite, sodium chloride produce fused salt grade sodium nitrate, it is characterised in that: including following step
It is rapid:
S01, the separation of sodium nitrite will be concentrated with the neutralizer of nitrogen oxides in soda ash, crystallize, nitrous acid is obtained by filtration
Sodium product and mother liquor A；
S02, the separation of chlorination magnesium addition, S01 obtain mother liquor A and nitric acid are added to convert, and remaining sodium nitrite is made all to generate nitric acid
Sodium, sodium nitrate solution liquid pass through 3-6 condensing crystallizing, it is isolated industry grade sodium nitrate and mother liquor B, mother liquor B in sodium chloride accumulate
Tiring out to the concentration of Cl- is 50-150g/L, and sodium chloride and sodium nitrate reach total saturation point under room temperature；Mother liquor B contains sodium chloride, chlorine
Change magnesium addition, the sodium carbonate with the amount of magnesium chloride same substance is added according to measurement, magnesium carbonate is settled out, through carbonic acid is obtained by filtration
Magnesium and filtrate；
S02 is obtained filtrate and continues to be concentrated by S03, the separation of sodium chloride as impurity, so that liquor capacity is reduced 20~30%, chlorination
When sodium crystallization is precipitated, continue to be heated to concentrate temperature to be 100-120 DEG C, the density of solution is 1.3~1.5Kg/L, NO3-'s
Concentration is that 380~500g/L is filtered, separating at high temperature sodium chloride is isolated when the concentration of Cl- is 70-110g/L
Hot mother liquor C crystallisation by cooling obtains nitric acid sodium crystal and cold mother liquor D, and cold mother liquor D is heated again to be concentrated and separated out sodium chloride, so follows
Sodium chloride and sodium nitrate are distinguished complete output by ring；
S04, recrystallization prepare fused salt grade sodium nitrate, and the industrial sodium nitrate that S02, S03 are obtained is female through first time condensing crystallizing in S02
Liquid water washing removes the sodium chloride of part attachment, isolates nitric acid sodium crystal, then dissolved with steam condensate (SC), recrystallized,
Isolated fused salt grade sodium nitrate and mother liquor E.
2. the method that accurate control separation sodium nitrite according to claim 1, sodium chloride produce fused salt grade sodium nitrate,
Be characterized in that: in the S01, the concentration be neutralizer is concentrated into sodium nitrate in solution concentration be 50~500g/
L, the crystallization be 10-60 DEG C at a temperature of carry out.
3. the method that accurate control separation sodium nitrite according to claim 1, sodium chloride produce fused salt grade sodium nitrate,
Be characterized in that: the concentration of the nitric acid in the S02 is 40%.
4. the method that accurate control separation sodium nitrite according to claim 1, sodium chloride produce fused salt grade sodium nitrate,
Be characterized in that: in the S04, the cleaning solution obtained after first time condensing crystallizing mother liquor water washing in S02 enters
The evaporation of sodium nitrate evaporator, control NO3 -Concentration be 380~500g/L, separating at high temperature goes out sodium chloride, the separation of filtrate crystallisation by cooling
Industrial nitric acid sodium crystal is obtained, into production system circular treatment, finally also obtains fused salt grade sodium nitrate.
5. the method that accurate control separation sodium nitrite according to claim 1, sodium chloride produce fused salt grade sodium nitrate,
It is characterized in that: in the S04, being recycled in the solution after mother liquor E is added to S02 plus nitric acid conversion.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115417433A (en) * | 2022-09-21 | 2022-12-02 | 成都市科隆化学品有限公司 | Method for producing high-purity sodium nitrate |
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