CN108675322A - A kind of purification process of sodium nitrate - Google Patents
A kind of purification process of sodium nitrate Download PDFInfo
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- CN108675322A CN108675322A CN201810908126.7A CN201810908126A CN108675322A CN 108675322 A CN108675322 A CN 108675322A CN 201810908126 A CN201810908126 A CN 201810908126A CN 108675322 A CN108675322 A CN 108675322A
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- chitosan
- sodium nitrate
- cobalt
- purification process
- adsorbing medium
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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
- 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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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of purification process of sodium nitrate.The purification process includes：Include the following steps：（1）The sodium nitrate solution of sodium nitrate crude product is set to pass through cobalt loading chitosan adsorbing medium；The wherein described cobalt loading chitosan adsorbing medium is to be impregnated in gained in cobalt nitrate solution by alkyl aldehydes cross-linked chitosan, and the alkyl cross-linked chitosan is to carry out the obtained cross-linked polymer of nucleophilic addition by the aldehyde radical of alkyl aldehydes and the amino of chitosan；（2）From through step（1）By isolating solid in liquid.In the purification process of the present invention, preferably sulfate radical foreign matter can be removed using cobalt loading chitosan adsorbing medium, effectively removed sulfate radical foreign matter in this way, ensure that the purity of product.
Description
Technical field
The present invention relates to the technical field of regent purification more particularly to a kind of purification process of sodium nitrate.
Background technology
Sodium nitrate, fusing point are 306.8 DEG C, and density is 2.257 grams/cc（At 20 DEG C）, it is water white transparency or white micro-
Band yellow rhomboidan.Its bitter is salty, and soluble easily in water and liquefied ammonia is slightly soluble in glycerine and ethyl alcohol, easily deliquesces.Porcelain enamel industry is used as
Fluxing agent, oxidant and the raw material for preparing enamel frit.Glass industry is used as the decolorising agent of various glass and product, defoaming
Agent, fining agent and oxidation fluxing agent.Inorganic industrial is used as the decolorising agent of molten caustic (soda) and for manufacturing other Nitrates.Food
Industry is used as the colour former of meat packing, meat can be prevented rotten, and can play seasoning.Chemical fertilizer industry is used as being applicable in acid soil
The quick-acting fertilizer of earth, particularly suitable root crop, such as beet, radish.Dye industry is used as the original of production bitter taste acid and direct dyes
Material.Heat treatment agent of the metallurgical industry as steel-making, aluminium alloy.The industry of machine city is used as metal cleaner and preparation ferrous metal turns blue
Agent.Medical industry is used as the culture medium of penicillin.Cigarette industry is used as the combustion adjuvant of tobacco.It is used as chemical examination in analytical chemistry
Agent.In addition, being also used for production explosive etc..
105271315 A of Chinese patent CN disclose a kind of method producing chemical products sodium nitrate, and this method is to use
The Ca (NO3) 2 and saltcake that the calcium carbonate mineral (especially calcite) of high-purity obtains after being reacted with nitric acid (HN03)
(Na2SO4) after reacting in the solution, it is first separated by filtration acid insoluble matter, then mistake under alkaline condition in acid condition
The alkaline insoluble matter of filter separation is finally pure using sodium nitrate produced by the invention by filtrate condensing crystallizing sodium nitrate (NaNO3)
Degree is high, and can produce by-product coating grade gypsum simultaneously, and high conversion rate is at low cost up to 95%, profitable.
For containing sulfate radical foreign matter in the product of the above sodium nitrate, the above method is purified by pickling, alkali cleaning,
The purification process can not effectively be only capable of preferably going to deacidify, and fail to effectively remove for sulfate radical, cause the purity of product not high.
Invention content
In view of this, the present invention provides a kind of purification process of sodium nitrate, the refined product obtained through the purification process is pure
Degree is higher.
The purification process of the sodium nitrate of the present invention, includes the following steps：
（1）The sodium nitrate solution of sodium nitrate crude product is set to pass through cobalt loading chitosan adsorbing medium；The wherein described cobalt loading chitosan
Adsorbing medium is to be impregnated in gained in cobalt nitrate solution by alkyl aldehydes cross-linked chitosan, and the alkyl cross-linked chitosan is by alkyl
The aldehyde radical of aldehyde and the amino of chitosan carry out the obtained cross-linked polymer of nucleophilic addition；
（2）From through step（1）By isolating solid in liquid.
Cobalt loading chitosan adsorbing medium
Cobalt loading chitosan adsorbing medium refers to by cobalt element by being chemically bound in chitosan molecule.Herein, it is chemically bonded
It is cobalt atom, chitosan-NH2Nitrogen-atoms formed coordinate bond.Compared to the chitosan that no cobalt loads, cobalt of the present invention is negative
Chitosan adsorbing medium is carried since the load of cobalt can significantly improve the adsorption capacity to sulfate ion, the reason is that：Cobalt is negative
Chitosan adsorbing medium is carried in forming process, cobalt ions in aqueous solution with the existence form of hydrate and chitosan-
NH2Form the complex with cobalt hydrate（It is that cobalt hydrate complexing cation forms coordinate bond with nitrogen in the complex）, institute
The complex molecule of formation is positively charged, so that originally neutral chitosan is become positively charged in this way, improves chitosan to sulfate radical
Adsorption capacity.Reaction process is as follows：
。
The preparation method of cobalt loading chitosan adsorbing medium is, molten using cobalt nitrate is impregnated in by alkyl aldehydes cross-linked chitosan
Gained in liquid.The pH of the dipping is preferably 2~4.If pH is too small, H+ can preferentially occupy leading position and then protonate shell
A NH2 in glycan molecule structure forms it into a NH3+, and then weaken the chelant ability of amino, therefore adsorbance is caused to compare
It is low.If pH is excessive, the cobalt ions loaded on cross-linked chitosan will appear the trend for gradually forming hydroxide precipitation and cause
Coordination cannot be carried out with adsorbent causes absorption to decline.The advantageous pH range of the present invention enables to adsorbance to reach maximum,
This is because the H+ and cobalt ions in system, in competition coordination, H ', which is constantly reduced, causes wrong ion to start to occupy advantage,
So that chelant ability increases, therefore the adsorption capacity of sulfate radical is enhanced.
The concentration of cobalt nitrate solution is preferably 150~400mg/L, in terms of cobalt quality.
The temperature of dipping can be 20~40 DEG C, and at a temperature of this, the time of dipping is 0.5~2h.
Preferably, the type of feed of the cobalt loading chitosan adsorbing medium is adsorption column.
Preferably, it is 50~100mL/min by the flow velocity of the adsorption column of cobalt loading chitosan adsorbing medium.
Alkyl aldehydes cross-linked chitosan
The alkyl aldehydes cross-linked chitosan of the present invention is that the amino progress nucleophilic addition of the aldehyde radical and chitosan of alkyl aldehydes is obtained
Cross-linked polymer.The equation of the nucleophilic addition is
Well known method can be used to obtain in the reaction condition of the nucleophilic addition, such as inverse suspension crosslinking method can be used, i.e., will
For chitosan dissolution of raw material in the acetic acid solution of 2wt%, sonic vacuum deaeration is spare：A certain amount of liquid is added in three-necked flask
Body paraffin and emulsifier span 80 stir a period of time under certain temperature, the chitosan solution got ready are then added to three mouthfuls
Continue to stir in flask, the liquid pearl that chitosan is dispersed into uniform particle sizes by w/o types system is formed by stirring;Then what is heated up is same
When be added various dose crosslinking agent glutaraldehyde, carry out cross-linking reaction;Use lye regulation system pH value to weak base after a certain period of time
Property, the reaction was continued a period of time；Product is used in combination solvent appropriate fully to wash for several times, will be washed through vacuum filter after reaction
Product vacuum after washing is drying to obtain glycan substrate.Certainly, it reference may also be made to Deng.
Step in the present invention（2）Described in that the mode of sodium nitrate solid is isolated from sodium nitrate solution is public using this field
All method for crystallising known, such as evaporative crystallization or decrease temperature crystalline etc..Such as reduced pressure, then decrease temperature crystalline can be heated first.
Herein, the pressure for heating reduced pressure be can be 0.08~0.12MPa, such as 0.08 MPa, 0.082MPa,
0.085MPa, 0.09MPa, 0.10MPa, 0.11MPa, 0.115MPa, 0.118MPa or 0.12MPa etc..What heating was concentrated under reduced pressure
Temperature can be 72~78 DEG C.
The temperature of decrease temperature crystalline can be 2~8 DEG C.
Above-mentioned sodium nitrate crude product can be used industrial grade sodium nitrate, and purity can be 95~97wt%, such as 95wt%,
95.5wt%, 96wt%, 96.5wt%, 96.8wt% or 97wt% etc..
The present invention does not address place and is suitable for the prior art.
As used herein, above-mentioned term：
" mass parts " refer to the basic measurement unit for the mass ratio relationship for indicating multiple components, and 1 part can indicate arbitrary unit matter
Amount, can such as be expressed as 1g, may also indicate that 2.689g etc..If we say that the mass parts of component A are a parts, the mass parts of B component
It it is b parts, then it represents that the quality of component A and the mass ratio a of B component：b.Or ground, indicate that the quality of component A is aK, B component
Quality be bK（K is arbitrary number, indicates multiplying factor）.It can not misread, unlike mass fraction, all components
The sum of mass parts are not limited to 100 parts of limitation.
"one", "an" and " described " be used interchangeably and refer to one or more.
"and/or" is used to indicate that one of illustrated situation or both may to occur, for example, A and/or B includes (A
And B) and (A or B).
In addition, the range stated herein by endpoint includes all numerical value for being included within the scope of this（For example, 1 to 10 packet
Include 1.4,1.9,2.33,5.75,9.98 etc.）.
In addition, the statement of "at least one" herein includes one or more all numbers（For example, at least two, at least
4, at least six, at least eight, at least ten, at least 25, at least 50, at least 100 etc.）.
In the purification process of the present invention, preferably sulfate radical foreign matter can be carried out using cobalt loading chitosan adsorbing medium
Removal, has effectively removed sulfate radical foreign matter, ensure that the purity of product in this way.
Specific implementation mode
The technical solution further illustrated the present invention with reference to embodiment.
Embodiment 1
It weighs a certain amount of chitosan to be put into the there-necked flask of 500 mL, is separately added into 30 mL carbon tetrachloride, 30 mL petroleum ethers
The dim aqueous acid of chitosan that 60 mL mass fractions are 5% is added, is stirred in 450rpm under electric stirring with 6 mL Span80
Speed is mixed, chitosan solution is separated into sizeable droplet after 40min, and it is molten that the formaldehyde that a certain amount of volume fraction is 37% is added dropwise
The glutaraldehyde solution that a certain amount of volume fraction is 50% is added dropwise after 60 min, obtains the chitosan microball of the different degrees of cross linking again for liquid.
Gelation is completed after 90 min, and the NaOH solution that mass fraction is 10% is added dropwise, and adjusts pH value to alkalescence.After 10 min, it is warming up to
60 DEG C of reaction 4h, make ball cure, and then filter and are washed to neutrality, with acetone extraction 3h, take out, are dried in vacuo to get formaldehyde-
Glutaraldehyde cross-linking chitosan microball.
It is placed in above-mentioned formaldehyde-glutaraldehyde cross-linking chitosan microball in the conical flask of 250 mL, it is centainly dense that 100 mL are added
The cobalt nitrate solution of degree, the constant temperature oscillation certain time at 20 DEG C, control pH are 2, and control hunting speed is 180 rpm.It waits soaking
It after stain 2h, centrifuges, filters, 24 h are dried in vacuo at 60 DEG C, obtain cobalt load formaldehyde-glutaraldehyde cross-linking chitosan absorption and be situated between
Matter.
The sodium nitrate crude product of 95wt% purity is dissolved in the water, sodium nitrate solution is formed, it is spare.
Cobalt load formaldehyde-glutaraldehyde cross-linking chitosan adsorbing medium of above-mentioned preparation is packed into adsorption column.And make
For sodium nitrate solution with the flow velocity of 150mg/L by the adsorption column, collection passes through liquid.
Sodium nitrate crystalline substance will be obtained above by liquid in 0.08MPa pressure, 72 DEG C of heating concentrations, then the crystallisation by cooling at 2 DEG C
Nitric acid sodium crystal is finally washed with deionized and is dried by body.
The purity 99.75% of the obtained sodium nitrate of the present embodiment（ICP-MS is analyzed）.
Embodiment 2
It weighs a certain amount of chitosan to be put into the there-necked flask of 500 mL, is separately added into 30 mL carbon tetrachloride, 30 mL petroleum ethers
The dim aqueous acid of chitosan that 60 mL mass fractions are 5% is added, is stirred in 450rpm under electric stirring with 6 mL Span80
Speed is mixed, chitosan solution is separated into sizeable droplet after 40min, and it is molten that the formaldehyde that a certain amount of volume fraction is 37% is added dropwise
The glutaraldehyde solution that a certain amount of volume fraction is 50% is added dropwise after 60 min, obtains the chitosan microball of the different degrees of cross linking again for liquid.
Gelation is completed after 90 min, and the NaOH solution that mass fraction is 10% is added dropwise, and adjusts pH value to alkalescence.After 10 min, it is warming up to
60 DEG C of reaction 4h, make ball cure, and then filter and are washed to neutrality, with acetone extraction 3h, take out, are dried in vacuo to get formaldehyde-
Glutaraldehyde cross-linking chitosan microball.
It is placed in above-mentioned formaldehyde-glutaraldehyde cross-linking chitosan microball in the conical flask of 250 mL, it is centainly dense that 100 mL are added
The cobalt nitrate solution of degree, the constant temperature oscillation certain time at 40 DEG C, control pH are 4, and control hunting speed is 180 rpm.It waits soaking
It after stain 0.5h, centrifuges, filters, 24 h are dried in vacuo at 60 DEG C, obtain cobalt load formaldehyde-glutaraldehyde cross-linking chitosan absorption and be situated between
Matter.
The sodium nitrate crude product of 97wt% purity is dissolved in the water, sodium nitrate solution is formed, it is spare.
Cobalt load formaldehyde-glutaraldehyde cross-linking chitosan adsorbing medium of above-mentioned preparation is packed into adsorption column.And make
For sodium nitrate solution with the flow velocity of 400mg/L by the adsorption column, collection passes through liquid.
Sodium nitrate crystalline substance will be obtained above by liquid in 0.12MPa pressure, 78 DEG C of heating concentrations, then the crystallisation by cooling at 8 DEG C
Nitric acid sodium crystal is finally washed with deionized and is dried by body.
The purity 99.83% of the obtained sodium nitrate of the present embodiment（ICP-MS is analyzed）.
Embodiment 3
It weighs a certain amount of chitosan to be put into the there-necked flask of 500 mL, is separately added into 30 mL carbon tetrachloride, 30 mL petroleum ethers
The dim aqueous acid of chitosan that 60 mL mass fractions are 5% is added, is stirred in 450rpm under electric stirring with 6 mL Span80
Speed is mixed, chitosan solution is separated into sizeable droplet after 40min, and it is molten that the formaldehyde that a certain amount of volume fraction is 37% is added dropwise
The glutaraldehyde solution that a certain amount of volume fraction is 50% is added dropwise after 60 min, obtains the chitosan microball of the different degrees of cross linking again for liquid.
Gelation is completed after 90 min, and the NaOH solution that mass fraction is 10% is added dropwise, and adjusts pH value to alkalescence.After 10 min, it is warming up to
60 DEG C of reaction 4h, make ball cure, and then filter and are washed to neutrality, with acetone extraction 3h, take out, are dried in vacuo to get formaldehyde-
Glutaraldehyde cross-linking chitosan microball.
It is placed in above-mentioned formaldehyde-glutaraldehyde cross-linking chitosan microball in the conical flask of 250 mL, it is centainly dense that 100 mL are added
The cobalt nitrate solution of degree, the constant temperature oscillation certain time at 20~40 DEG C, control pH are 3, and control hunting speed is 180 rpm.
It after 1h to be impregnated, centrifuges, filters, 24 h are dried in vacuo at 60 DEG C, obtain cobalt load formaldehyde-glutaraldehyde cross-linking chitosan absorption
Medium.
The sodium nitrate crude product of 96wt% purity is dissolved in the water, sodium nitrate solution is formed, it is spare.
Cobalt load formaldehyde-glutaraldehyde cross-linking chitosan adsorbing medium of above-mentioned preparation is packed into adsorption column.And make
For sodium nitrate solution with the flow velocity of 300mg/L by the adsorption column, collection passes through liquid.
Sodium nitrate crystalline substance will be obtained above by liquid in 0.10MPa pressure, 75 DEG C of heating concentrations, then crystallisation by cooling at 5 DEG C
Nitric acid sodium crystal is finally washed with deionized and is dried by body.
The purity 99.95% of the obtained sodium nitrate of the present embodiment（ICP-MS is analyzed）.
Embodiment 4
It weighs a certain amount of chitosan to be put into the there-necked flask of 500 mL, is separately added into 30 mL carbon tetrachloride, 30 mL petroleum ethers
The dim aqueous acid of chitosan that 60 mL mass fractions are 5% is added, is stirred in 450rpm under electric stirring with 6 mL Span80
Speed is mixed, chitosan solution is separated into sizeable droplet after 40min, and it is molten that the formaldehyde that a certain amount of volume fraction is 37% is added dropwise
The glutaraldehyde solution that a certain amount of volume fraction is 50% is added dropwise after 60 min, obtains the chitosan microball of the different degrees of cross linking again for liquid.
Gelation is completed after 90 min, and the NaOH solution that mass fraction is 10% is added dropwise, and adjusts pH value to alkalescence.After 10 min, it is warming up to
60 DEG C of reaction 4h, make ball cure, and then filter and are washed to neutrality, with acetone extraction 3h, take out, are dried in vacuo to get formaldehyde-
Glutaraldehyde cross-linking chitosan microball.
It is placed in above-mentioned formaldehyde-glutaraldehyde cross-linking chitosan microball in the conical flask of 250 mL, it is centainly dense that 100 mL are added
The cobalt nitrate solution of degree, the constant temperature oscillation certain time at 30 DEG C, control pH are 2, and control hunting speed is 180 rpm.It waits soaking
It after stain 1h, centrifuges, filters, 24 h are dried in vacuo at 60 DEG C, obtain cobalt load formaldehyde-glutaraldehyde cross-linking chitosan absorption and be situated between
Matter.
The sodium nitrate crude product of 96wt% purity is dissolved in the water, sodium nitrate solution is formed, it is spare.
Cobalt load formaldehyde-glutaraldehyde cross-linking chitosan adsorbing medium of above-mentioned preparation is packed into adsorption column.And make
For sodium nitrate solution with the flow velocity of 400mg/L by the adsorption column, collection passes through liquid.
Sodium nitrate crystalline substance will be obtained above by liquid in 0.10MPa pressure, 75 DEG C of heating concentrations, then crystallisation by cooling at 5 DEG C
Nitric acid sodium crystal is finally washed with deionized and is dried by body.
The purity 99.90% of the obtained sodium nitrate of the present embodiment（ICP-MS is analyzed）.
Since the numberical range of each technological parameter involved in the present invention can not possibly all embody in the above-described embodiments,
As long as but those skilled in the art's envisioned any numerical value fallen into the above-mentioned numberical range completely can implement this
Invention also includes the arbitrary combination of occurrence in several numberical ranges certainly.Herein, for length the considerations of, be omitted to
Go out the embodiment of occurrence in certain one or more numberical range, this disclosure for being not to be construed as technical scheme of the present invention is not filled
Point.
Applicant states that the present invention illustrates detailed process equipment and the technological process of the present invention by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological processes, that is, it is above-mentioned detailed not mean that the present invention has to rely on
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
The addition of equivalence replacement and auxiliary element to each raw material of product of the present invention, the selection etc. of concrete mode all fall within the present invention's
Within protection domain and the open scope.
Claims (7)
1. a kind of purification process of sodium nitrate, which is characterized in that include the following steps：
（1）The sodium nitrate solution of sodium nitrate crude product is set to pass through cobalt loading chitosan adsorbing medium；The wherein described cobalt loading chitosan
Adsorbing medium is to be impregnated in gained in cobalt nitrate solution by alkyl aldehydes cross-linked chitosan, and the alkyl cross-linked chitosan is by alkyl
The aldehyde radical of aldehyde and the amino of chitosan carry out the obtained cross-linked polymer of nucleophilic addition；
（2）From through step（1）By isolating solid in liquid.
2. purification process according to claim 1, which is characterized in that step（1）Described in the pH that impregnates be 2~4.
3. the purification process stated according to claim 1, which is characterized in that step（1）Described in cobalt nitrate solution a concentration of 150
~400mg/L, in terms of cobalt quality.
4. the purification process stated according to claim 1, which is characterized in that step（1）Described in the temperature that impregnates be 20~40 DEG C,
The time of dipping is 0.5~2h.
5. purification process according to claim 1, which is characterized in that the filling side of the cobalt loading chitosan adsorbing medium
Formula is adsorption column.
6. the purification process stated according to claim 5, which is characterized in that step（1）In pass through cobalt loading chitosan adsorbing medium
Adsorption column flow velocity be 50~100mL/min.
7. purification process according to claim 1, which is characterized in that step（2）Described in detached from sodium nitrate solution
The mode for going out sodium nitrate solid is heating reduced pressure, then decrease temperature crystalline.
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| CN201810908126.7A CN108675322A (en) | 2018-08-10 | 2018-08-10 | A kind of purification process of sodium nitrate |
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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 |
Citations (1)
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| CN106146913A (en) * | 2015-04-21 | 2016-11-23 | 南方科技大学 | A kind of chitosan-based hydrogel and its preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106146913A (en) * | 2015-04-21 | 2016-11-23 | 南方科技大学 | A kind of chitosan-based hydrogel and its preparation method and application |
Non-Patent Citations (1)
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Cited By (2)
| 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 |
| CN115417433B (en) * | 2022-09-21 | 2024-04-12 | 成都市科隆化学品有限公司 | Method for producing high-purity sodium nitrate |
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