CN105271315A - Novel method for producing sodium nitrate from mirabilite - Google Patents
Novel method for producing sodium nitrate from mirabilite Download PDFInfo
- Publication number
- CN105271315A CN105271315A CN201510847622.2A CN201510847622A CN105271315A CN 105271315 A CN105271315 A CN 105271315A CN 201510847622 A CN201510847622 A CN 201510847622A CN 105271315 A CN105271315 A CN 105271315A
- Authority
- CN
- China
- Prior art keywords
- nitrocalcite
- carry out
- acid
- sodium nitrate
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a novel method for producing sodium nitrate from mirabilite. The novel method comprises the following steps: reacting high-purity calcium carbonate ore (particularly calcite) and nitric acid (HNO3) to react to obtain Ca(NO3), enabling Ca(NO3) and mirabilite (Na2SO4) in a solution, filtering under an acid condition to separate acid undissolved substances, furthermore filtering under an alkali condition to separate alkali undissolved substances, and finally concentrating and crystallizing the filtrate, thereby obtaining sodium nitrate (NaNO3). By adopting the novel method, the sodium nitrate is high in purity, a byproduct coating grade gypsum can be simultaneously prepared, the conversion rate is as high as 95%, the cost is low, and good benefits can be made.
Description
The present invention is a kind of method of production chemical product SODIUMNITRATE.
At present, the processing method of production SODIUMNITRATE in the world has following several: one is Chile, utilizes that sodium nitrate is broken to be got; Two is the U.S., utilizes Sweet natural gas and caustic soda to break and is combined to; Three is that other countries utilize nitric acid and soda ash neutralization to form.
Before making the present invention, contriver's experiment be at first with in common lime and nitric acid and obtained nitrocalcite liquid and saltcake solution react, then filter, concentrate, crystallization sodium nitrate.But purity does not reach technical grade standard, by-produced gypsum can not be made coating and use.After completing the present invention, contriver learns Nei Youliangge county of Sichuan Province, have employed the operational path that the intermediate product nitrocalcite prepared with superfluous lime and nitric acid reaction reacts with saltcake, filters, concentrates, crystallization obtains SODIUMNITRATE and builds up factory, but not success.And the by product gypsum obtained can not do coating use, can only press plasterboard.Gansu Provincial Chemical Industry Inst. comrade Zhang Pingjun is published in " inorganic industrial salt " the 6th phase in 1986 upper " the in-problem research of double decomposition process for producing sodium nitrate ", also superfluous lime and nitric acid reaction is used, first filter at PH11-13, removing magnesium ion, when being acidified to PH2-3 again and saltcake react, adding a small amount of soda ash after question response completes adjusts PH to 7, filter, concentrated, the processing method of crystallization, there is its defective, he again this file this technique of being just grown up at the first bruss there are most distinct issues and be, product SODIUMNITRATE be separated in several first mixture, easily bring Ca (NO into
3)
2, Mg (NO
3)
2and CaSO
4with Ca (OH)
2deng impurity, and productive rate is low.Can not eliminate these impurity in theory with in practice by his working method, by product gypsum can not be made coating gypsum and use.
The object of the invention is.Utilize me to cross saltcake in highly purified calcium carbonate mineral, particularly calcite and saltings, northwest each province, produce to meet and use and the high purity SODIUMNITRATE of industry needs, work together and obtain coating and gypsum.
The present invention is a kind of according to CaCO
3+ 2HNO
3=Ca (NO
3)+H
2o+CO
2↑ and Ca (NO
3)+Na
2sO
4=CaSO ↓ NaNO
3ultimate principle, prepare the acidic solution of intermediate product nitrocalcite again after saltcake solution react with highly purified calcium carbonate mineral (especially calcite) and nitric acid reaction, first filter in acid condition, be separated acid insolubles, then containing Na
2cO
3alkaline condition under filtering separation alkalescence insolubles, finally by filtrate, concentrated, crystallization obtains the method for SODIUMNITRATE crystal.
Technical scheme of the present invention is:
1. prepare the acidic solution of intermediate product nitrocalcite, with highly purified calcium carbonate mineral particularly calcite, clean its impurity and earth with water, be placed in acidproof pond and add nitric acid, after reaction, obtain the acidic solution of nitrocalcite.Filtering clarifying liquid when preferably getting PH1-2 is for subsequent use.
2. the pre-treatment of saltcake.The cold saturated saltcake solution of saltcake crystal is washed away experiment and other impurity, then dissolving clarification is for subsequent use.
3. in acidproof pond, carry out the replacement(metathesis)reaction of nitrocalcite and saltcake, stir, heat, mixture is fully reacted.
4. look into the pH value of reaction solution with PH test paper, filter when particularly pH value is 6 to acidity, be separated acid insolubles.Filtrate adds nitrate of baryta reagent, knows and no longer produces till throw out, thoroughly goes out sulfate ion, and treating pond of filtrate being made a gift to someone after filtering separation throw out, completes acid filtration.
5., with the acid insolubles of water repetitive scrubbing, filtration, drying, obtain byproduct coating and gypsum, wash water is for diluting saltcake.
6. in treating pond solution, add calcined soda for industry, and after being stirred in solution alkaline, particularly during PH8-9, filtering separation precipitates, and completes purification.It is for subsequent use that scavenging solution sends into the clarification of storage pond.
7. the solution stored up in pond sends into evaporating pan, is concentrated into and just has xln to fold, proceed to crystallizing pond naturally cooling, carry out first time crystallization, crystal is pulled out, after rinsing with the sodium nitrate solution after a small amount of purification, send kiln dry, packaging can obtain food grade SODIUMNITRATE (NaNO
3) product.
8. the mother liquor after first time crystallization is proceeded to evaporating pan, be concentrated into mass crystallization and folded, proceeded to crystallizing pond naturally cooling, carry out second time crystallization, pull crystal out, send kiln drying after rinsing with the SODIUMNITRATE liquid after a small amount of purification, pack, obtain technical grade SODIUMNITRATE product.
Key problem in technology of the present invention is 1. to select highly purified calcium carbonate mineral, improves the purity of intermediate product nitrocalcite, requires CaCO in ore
3content is not less than 95%, preferably selects calcite.2., after replacement(metathesis)reaction, first is not that about PH6 comes in acidity, and be separated acid insolubles, and thoroughly remove sulfate ion, colleague in turn ensure that gypsum reaches coating grade standard.3. adjust pH value to reach alkalescence with soda ash acid for Ex-all filtrate that is not tolerant and sulfate ion, preferably make PH be 8-9, make the heavy metal ion of acid-soluble and calcium, magnesium, iron, barium plasma form insoluble hydrochloride, filtration can remove all dirt.
The closely-related prior art of the present invention is the basic solution with the nitrocalcite obtained after excessive common lime and nitric acid reaction.Filter after acidifying again with, saltcake reacts, then adjusts PH to filter to neutrality with soda ash.Finally filtrate is concentrated, crystallization sodium nitrate.Without obtaining successfully key, this method cannot be that common lime contains a large amount of impurity being difficult to remove, the intermediate product nitrocalcite purity of production is low.In addition, milk of lime is a kind of alkaline oxyhydroxide, and the alkali of some amphoteric metals can be made under its effect to produce the compound salt of the alkaline ca nitrate soln of energy honor.After acidifying, these compound salt form again the nitrate of solubility.Be difficult to this partial impurities of removing like this, thionic acid radical ion all cannot thoroughly remove.Remove carbonate deposition in neutral conditions, thoroughly cannot remove all metal ions in practice.So this several first mixture solution is carrying out a kind of metathetic reversible reaction all the time.Therefore this prior art also exists the difficulty of removing impurity and separating impurity, and has productive rate low, and by product gypsum can not be used as the shortcoming of coating.
The present invention compared with prior art, solves an above-mentioned difficult problem well, not only can the food grade of high-purity and the SODIUMNITRATE product of technical grade, and can provide marketed coating level gypsum simultaneously, and transformation efficiency can reach more than 95%.This special positively effect is that any method of prior art all cannot be accomplished.
Realizing preferred plan of the present invention is: by method of the present invention, select the nitrocalcite intermediate product of calcite and preparation of nitric acid, when pH value is 1-2 and saltcake solution mix and blend, and filter at PH6, be separated coating level gypsum, instillation nitrate of baryta thoroughly removes sulfate ion, PH8-9 is adjusted again with technical grade soda ash, nearly all metal ion and calcium, magnesium, barium, iron plasma is made to form carbonate deposition, a kind of highly purified sodium nitrate solution is obtained after filtration, by crystallization and purification, ensure that the purity of product SODIUMNITRATE.Contriver adopts this scheme, scale up test 500 kilograms of SODIUMNITRATE under the supervision of the Tongnan County State Scientific and Technological Commission.Through inspection, product is played card GB4553-84 mono-class primary standard.
Claims (8)
1. a production SODIUMNITRATE (NaNO
3) method, it is according to Ca (NO
3)
2na
2sO
4=CaSO
4↓+2NaNO
3ultimate principle, adopt the method for filtration, condensing crystal, feature of the present invention is, after the nitrocalcite obtained by highly purified calcium carbonate mineral and nitric acid reaction reacts in the solution with saltcake, first carry out acidity to filter, carry out alkaline filter again, finally filtrate condensing crystal is obtained SODIUMNITRATE crystal.
2. the method for claim 1, is characterized in that the calcium carbonate mineral purity for the preparation of nitrocalcite is not less than 95%.
3. the method for claim 1, is characterized in that for the preparation of the calcium carbonate mineral of nitrocalcite be calcite.
4. the method for claim 1, to it is characterized in that preparing nitrocalcite be a kind of acidic solution, particularly PJ value containing free nitric acid is the acidic solution of 1-2.
5. the method for claim 1, is characterized in that acid filtration is about 6 to carry out at pH value.
6. the method for claim 1, adds nitrate of baryta after it is characterized in that acid filtration, thoroughly eliminates sulfate ion.
7. the method for claim 1, is characterized in that alkaline filter is after completing acid filtration, adds after calcined soda for industry makes solution alkaline and carry out, particularly carry out when pH value 8-9.
8. the method for claim 1, is characterized in that acidity to filter after gained insolubles washes with water to obtain byproduct coating level gypsum.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510847622.2A CN105271315A (en) | 2015-11-27 | 2015-11-27 | Novel method for producing sodium nitrate from mirabilite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510847622.2A CN105271315A (en) | 2015-11-27 | 2015-11-27 | Novel method for producing sodium nitrate from mirabilite |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105271315A true CN105271315A (en) | 2016-01-27 |
Family
ID=55141254
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510847622.2A Pending CN105271315A (en) | 2015-11-27 | 2015-11-27 | Novel method for producing sodium nitrate from mirabilite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105271315A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112834687A (en) * | 2019-11-22 | 2021-05-25 | 河海大学 | Method for measuring content of combined chloride ions in concrete in chloride and sulfate coexisting environment |
-
2015
- 2015-11-27 CN CN201510847622.2A patent/CN105271315A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112834687A (en) * | 2019-11-22 | 2021-05-25 | 河海大学 | Method for measuring content of combined chloride ions in concrete in chloride and sulfate coexisting environment |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CA2756763C (en) | Process for simultaneous production of potassium sulphate, ammonium sulfate, magnesium hydroxide and/or magnesium oxide from kainite mixed salt and ammonia | |
| CA2851786C (en) | Processing of lithium containing material | |
| US11465907B2 (en) | Process for producing a concentrated aqueous sodium hydroxide solution | |
| CA2832509C (en) | Method for processing and utilizing bypass dusts obtained during the production of cement | |
| CN107814370B (en) | Circulating environment-friendly process method for preparing phosphate concentrate, product and application thereof | |
| JP5336408B2 (en) | Recovery of sodium chloride and other salts from brine | |
| IL176482A (en) | Process for recovery of sulphate of potash | |
| JP2005537202A (en) | Recovery of sodium chloride and other salts from brine | |
| CN110092396A (en) | A kind of method and system of graphene Waste Sulfuric Acid recycling | |
| SI20525A (en) | Method of producing potassium sulfate | |
| CN102328947B (en) | Method for recovering strontium slag | |
| WO2010125205A1 (en) | Method for producing ferrous sulphate from pyrite ash | |
| CN104787782B (en) | Produce industrial potassium nitrate and calcium sulfate technique | |
| MX2012000137A (en) | Process for production of commercial quality potassium nitrate from polyhalite. | |
| CN105271315A (en) | Novel method for producing sodium nitrate from mirabilite | |
| CN103896313A (en) | Method for preparing high-activity magnesium oxide by adopting old brine in salt lake as material | |
| US2758912A (en) | Process for producing a substantially sulfate-free and potassium-free magnesium chloride solution | |
| CN111392754B (en) | Method and equipment for purifying calcium chloride from fluorine-containing solid waste | |
| CN105565346A (en) | Novel method for producing sodium nitrate from saltcake | |
| CN87103218A (en) | Novel method with saltcake production SODIUMNITRATE | |
| DE10154004A1 (en) | Recovery of magnesium hydroxide and gypsum from natural or artificial brine, e.g. end liquor from potash works, uses ammonia or ammonium hydroxide for precipitation of magnesium hydroxide | |
| RU2513652C2 (en) | Method of obtaining magnesium oxide | |
| KR20040086327A (en) | A process for recovery of low sodium salt from bittern | |
| CN102862997A (en) | Method for removing magnesium and sulfate ion in salt lake brine of hexahydric salt-water system | |
| AU2010264079A1 (en) | Polyhalite IMI process for KNO3 production |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160127 |
|
| WD01 | Invention patent application deemed withdrawn after publication |