CN87103218A - Novel method with saltcake production SODIUMNITRATE - Google Patents
Novel method with saltcake production SODIUMNITRATE Download PDFInfo
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- CN87103218A CN87103218A CN 87103218 CN87103218A CN87103218A CN 87103218 A CN87103218 A CN 87103218A CN 87103218 CN87103218 CN 87103218 CN 87103218 A CN87103218 A CN 87103218A CN 87103218 A CN87103218 A CN 87103218A
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- sodiumnitrate
- nitrocalcite
- acid
- solution
- saltcake
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Abstract
The present invention is a kind of method of production chemical product SODIUMNITRATE.
The present invention adopts highly purified calcium carbonate mineral (particularly calcite) and nitric acid (HNO
3) Ca (NO that obtains after the reaction
3)
2, with saltcake (Na
2SO
4) in solution, react after, the first acid insolubles of filtering separation under acidic conditions, filtering separation alkalescence insolubles under alkaline condition is produced SODIUMNITRATE (NaNO with the filtrate condensing crystal at last again
3).
The SODIUMNITRATE purity height that adopts the present invention to produce, and can produce by product coating level gypsum simultaneously, transformation efficiency is up to 95%, and cost is low, and is profitable.
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: the one, and Chile utilizes that sodium nitrate is broken to be got; The 2nd, the U.S. utilizes Sweet natural gas and caustic soda to break and is combined to; The 3rd, other countries utilize nitric acid and soda ash neutralization to form.
Before the present invention, contriver's test at first is to react with saltcake solution with the nitrocalcite liquid that the neutralization of common lime and nitric acid makes, and filters then, concentrates, crystallization produces SODIUMNITRATE.But purity does not reach the technical grade standard, and by-produced gypsum can not be made the coating gypsum and use.After finishing the present invention, the contriver learns two counties in the Sichuan Province, has adopted the intermediate product nitrocalcite with superfluous lime and nitric acid reaction preparation to build up factory with saltcake reaction, filtration, operational path concentrated, that crystallization obtains SODIUMNITRATE, but not success.And the by product gypsum that obtains can not make coating and use, and can only press plasterboard.The comrade of Zhang Ping army of Gansu Provincial Chemical Industry Inst. was published in " inorganic chemicals industry " 1986 the 6th phases last " the in-problem research of double decomposition process for producing sodium nitrate ", also use superfluous lime and nitric acid reaction, filter at PH11-13 earlier, remove magnesium ion, when being acidified to PH2-3 again and saltcake reaction, the intact back of question response adds a small amount of soda ash and transfers PH to 7, filtration, concentrated, crystalline processing method, and the scarce sex-limited of it arranged.He just admits at the first bruss that at this article it is that the products obtained therefrom SODIUMNITRATE is separated, and easily brings Ca(NO into that there are distinct issues in this technology in several first mixtures
3)
2, Mg(NO
3)
2, and CaSO
4And Ca(OH)
2Deng impurity, and productive rate is low.Working method by him can not eliminate these impurity in theory with in the practice, and the by product gypsum can not be made the coating gypsum and use.
The objective of the invention is, utilize China highly purified calcium carbonate mineral, particularly calcite,, produce the highly purified SODIUMNITRATE that satisfies edible and industrial needs, obtain coating level gypsum simultaneously with the saltcake in the saltings, each province, northwest.
The present invention is a kind of basis
Ultimate principle, prepare the acidic solution of intermediate product nitrocalcite with highly purified calcium carbonate mineral (especially calcite) and nitric acid reaction, again with the saltcake solution reaction after, under acidic conditions, filter earlier, separate acid insolubles, containing Na again
2CO
3Alkaline condition under filtering separation alkalescence insolubles, at last filtrate is concentrated, crystallization obtains SODIUMNITRATE crystalline method.
Technical scheme of the present invention is:
1, the acidic solution of preparation intermediate product nitrocalcite with highly purified calcium carbonate mineral calcite particularly, to wash clean its impurity and earth, places adding nitric acid acidproof pond in, obtains the acidity appearance liquid of nitrocalcite after the reaction.Filtering clarifying liquid when preferably getting PH1-2 is standby.
2, the pre-treatment of saltcake.With cold saturated saltcake solution flush away salt and other impurity, the dissolving clarification is standby again with the saltcake crystal.
3, in acidproof pond, carry out the replacement(metathesis)reaction of nitrocalcite and saltcake, stir, heat, mixture is fully reacted.
4, look into the reaction solution pH value with the PH test paper, acidity particularly pH value be to filter in 6 o'clock, separate acid insolubles, filtrate adds nitrate of baryta reagent, till no longer producing throw out, thoroughly removes sulfate ion, behind the filtering separation throw out filtrate is sent into treating pond, finish acid the filtration.
5, the acid insolubles of water repetitive scrubbing, filtration, drying obtain byproduct coating level gypsum, and wash water is used to dilute saltcake.
6, add calcined soda for industry in treating pond solution, and after being stirred in solution and being alkalescence, particularly during PH8-9, the filtering separation precipitation is finished purification, and it is standby that scavenging solution is sent into the Chu Chi clarification.
7, the solution in the storage pond is sent into evaporating pan, being concentrated into just has xln to fold, and changes the crystallizing pond naturally cooling over to, carries out the crystallization first time.Crystal is pulled out, after the sodium nitrate solution flushing after a small amount of the purification, sent the kiln drying, packing can obtain food grade SODIUMNITRATE (NaNO
3) product.
8, the mother liquor after the crystallization is for the first time changed over to evaporating pan, be concentrated into mass crystallization and separated out, change the crystallizing pond naturally cooling over to, carry out the crystallization second time, pull crystal out,, obtain technical grade SODIUMNITRATE product with sending the kiln drying after the SODIUMNITRATE liquid flushing after a small amount of the purification, packing.
Key problem in technology of the present invention is 1. to select for use highly purified calcium carbonate mineral, improves the purity of intermediate product nitrocalcite, requires CaCO in the ore
3Content is not less than 95%, preferably selects calcite for use.2. after the replacement(metathesis)reaction, particularly filter about PH6 in acidity earlier, separate acid insolubles, and thoroughly remove sulfate ion, guaranteed that again gypsum reaches the coating grade standard simultaneously.3. transfer the filtrate of acid insolubles of Ex-all and sulfate ion pH value to reach alkalescence with soda ash, preferably making PH is 8-9, makes acid soluble heavy metal ion and calcium, magnesium, iron, barium plasma form insoluble carbonate, and filtration can be removed all dirt.
With the closely-related prior art of the present invention, it is basic solution with the nitrocalcite that obtains behind excessive common lime and the nitric acid reaction, react with saltcake after filtering acidifying again, transfer PH to filter to neutrality with soda ash again, SODIUMNITRATE is produced at last that filtrate is concentrated, crystallization.The key that this method can't be succeedd is that common lime contains a large amount of impurity that is difficult to remove, and the intermediate product nitrocalcite purity of production is low.In addition, milk of lime is a kind of strong basicity oxyhydroxide, can make the alkali of some amphoteric metals produce the compound salt that can be dissolved in alkaline ca nitrate soln under its effect.After the acidifying, these compound salt form the nitrate of solubility again.Be difficult to remove this a part of impurity like this, the thionic acid radical ion all can't thoroughly be removed.Under neutrallty condition, remove carbonate deposition, can't thoroughly 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 exists the difficulty of removing impurity and separating impurity, and has productive rate low, the shortcoming that the by product gypsum can not be used as coating.
The present invention compared with prior art, solved an above-mentioned difficult problem well, not only can produce highly purified food grade and technical grade SODIUMNITRATE product, and can provide marketed coating level gypsum simultaneously, transformation efficiency can reach more than 95%, and this special positively effect is that any method of prior art all can't be accomplished.
Realize that preferred plan of the present invention is: by method of the present invention, select the nitrocalcite intermediate product of calcite and nitric acid preparation for use, when being 1-2, pH value mixes stirring with saltcake solution, and filter at PH6, separate coating level gypsum, splash into nitrate of baryta and thoroughly remove sulfate ion, transfer PH8-9 with technical grade soda ash again, make nearly all heavy metal ion and calcium, magnesium, barium, iron ion form carbonate deposition, obtain a kind of highly purified sodium nitrate solution after the filtration, by crystallization and purification, guaranteed the purity of product SODIUMNITRATE.The contriver adopts this scheme, has produced 500 kilograms of SODIUMNITRATE as a trial under the supervision of the Tongnan County State Scientific and Technological Commission, and through check, product reaches GB4553-84 one class primary standard.
Claims (8)
1, a kind of production SODIUMNITRATE (NaNO
3) method, it is according to Ca (NO
3)
2+ Na
2SO
4=CaSO
4↓+2NaNO
3Ultimate principle, adopt filtration, concentrated, crystalline method, feature of the present invention is, after the nitrocalcite that obtains with highly purified calcium carbonate mineral and nitric acid reaction reacts in solution with saltcake, carrying out acidity earlier filters, carry out alkaline filter again, at last the filtrate condensing crystal is obtained the SODIUMNITRATE crystal.
2, the method for claim 1, the calcium carbonate mineral purity that it is characterized in that being used to preparing nitrocalcite is not less than 95%.
3, the method for claim 1, the calcium carbonate mineral that it is characterized in that being used to preparing nitrocalcite is a calcite.
4, the method for claim 1 is characterized in that the nitrocalcite for preparing is that a kind of acidic solution, particularly pH value that contains free nitric acid is the acidic solution of 1-2.
5, the method for claim 1 is characterized in that acid the filtration is to be about 6 to carry out at pH value.
6, the method for claim 1 is characterized in that the acid back of filtering adds nitrate of baryta, thoroughly eliminates sulfate ion.
7, the method for claim 1 is characterized in that alkaline filter is after finishing acid the filtration, adds to carry out after calcined soda for industry makes solution be alkalescence, particularly carries out when pH value 8-9.
8, the method for claim 1 is characterized in that acidity filtered and obtains byproduct coating level gypsum after the gained insolubles washes with water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 87103218 CN87103218A (en) | 1987-04-26 | 1987-04-26 | Novel method with saltcake production SODIUMNITRATE |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 87103218 CN87103218A (en) | 1987-04-26 | 1987-04-26 | Novel method with saltcake production SODIUMNITRATE |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN87103218A true CN87103218A (en) | 1988-11-23 |
Family
ID=4814337
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 87103218 Pending CN87103218A (en) | 1987-04-26 | 1987-04-26 | Novel method with saltcake production SODIUMNITRATE |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN87103218A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101306822B (en) * | 2007-05-15 | 2010-09-15 | 新疆硝石钾肥有限公司 | NaNO3 leaching liquid prepared saltier ore |
| CN104150456A (en) * | 2014-08-13 | 2014-11-19 | 连云港市德邦精细化工有限公司 | Method for producing calcium phosphate salt and sodium phosphate salt by using sodium sulfate wastewater |
-
1987
- 1987-04-26 CN CN 87103218 patent/CN87103218A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101306822B (en) * | 2007-05-15 | 2010-09-15 | 新疆硝石钾肥有限公司 | NaNO3 leaching liquid prepared saltier ore |
| CN104150456A (en) * | 2014-08-13 | 2014-11-19 | 连云港市德邦精细化工有限公司 | Method for producing calcium phosphate salt and sodium phosphate salt by using sodium sulfate wastewater |
| CN104150456B (en) * | 2014-08-13 | 2016-06-08 | 连云港市德邦精细化工有限公司 | The method producing synthos and sodium ascorbyl phosphate with sodium sulfate wastewater |
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| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |