CN103496718B - Method for improving concentration of sodium hydroxide and method for improving concentration and purity of sodium hydroxide - Google Patents
Method for improving concentration of sodium hydroxide and method for improving concentration and purity of sodium hydroxide Download PDFInfo
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- CN103496718B CN103496718B CN201310459578.9A CN201310459578A CN103496718B CN 103496718 B CN103496718 B CN 103496718B CN 201310459578 A CN201310459578 A CN 201310459578A CN 103496718 B CN103496718 B CN 103496718B
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- sodium hydroxide
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Abstract
The invention provides a method for improving the concentration of sodium hydroxide and a method for improving concentration and purity of sodium hydroxide. The method for improving the concentration of sodium hydroxide comprises the following steps: adding a sodium alkoxide compound to the sodium hydroxide solution to be treated, and thus generating organic alcohol and sodium hydroxide through the hydrolysis reaction between the sodium alkoxide compound and water in the sodium hydroxide solution to be treated; after completely reacting, distilling so as to removal the organic alcohol, thus obtaining the sodium hydroxide finished product. The method can be used for improving the concentration of sodium hydroxide and removing part of impurities. Compared with a direct distillation method, the method has the advantages that the time is greatly saved, and the cyclic utilization of sodium hydroxide is facilitated.
Description
Technical field
The present invention relates to chemical technology field, more particularly, relate to a kind of method improving naoh concentration.
Background technology
Sodium hydroxide is conventional chemical reagent, and general industry adopts electrolysis NaCl on producing
2method preparation, Ca(OH also can be used in laboratory)
2+ NaCO
3+ H
2o → NaOH+CaCO
3↓ method obtain.Sodium hydroxide solution wherein reaches the concentration range of needs through evaporation concentration.
At present, industrially sodium hydroxide concentration after using reduces, and the way of recycle is the sodium hydroxide solution be recovered to is carried out evaporation concentration, to obtain the sodium hydroxide solution requiring concentration range.The following problem of above-mentioned technique ubiquity: (1) evaporation concentration amount is large; (2) consume energy high; (3) cycle is long, and efficiency is low; (4) recycle is loaded down with trivial details.
Publication number is that the Chinese patent of CN1792799A discloses a kind of method improving producing aluminium oxide circulating efficiency by Bayer process.The extraction agent such as alkylphenol, fluorinated alcohols that the method adopts n-Octanol, C6-C20 fatty alcohol or their mixture, carbon chain lengths is C13-C18 extracts sodium hydroxide from Bayer process circulation fluid, and then goes out sodium hydroxide with water back extraction.
The Chinese patent of publication number CN1923694A discloses the sodium hydroxide process of the sodium aluminate solution in the production of extractive distillation separation of oxygenated aluminium.The method adopts fatty alcohol to make extraction agent, sodium hydroxide in extraction sodium aluminate solution, as the caustic alkali in mother liquid evaporation, raffinate returning alumina production system after extraction, carry out decomposition of crystal seed, extraction phase decomposition nut liquid or aluminum hydroxide wash liquor or water back extraction, the aqueous phase solution after back extraction enters alumina producing system, oil phase continues on for extraction, oil phase continuous circulation like this after Distallation systm distillation.
Above-mentioned two patents are and adopt extraction agent directly to extract sodium hydroxide in organic phase, then adopt water or other dilute solution from organic phase sodium hydroxide back extraction out, obtain the aqueous solution of sodium hydroxide or contain other dilute solution of sodium hydroxide, complex process.
Summary of the invention
For the deficiencies in the prior art, an object of the present invention is to solve in above-mentioned prior art the one or more problems existed.
An object of the present invention is to provide a kind of method that can improve concentration of sodium hydroxide solution efficiently.
To achieve these goals, an aspect of of the present present invention provides a kind of method improving naoh concentration.Said method comprising the steps of: in pending sodium hydroxide solution, add alcohol sodium compound, the water generation hydrolysis reaction in described alcohol sodium compound and pending sodium hydroxide solution generates Organic Alcohol and sodium hydroxide; After question response is complete, Organic Alcohol is removed in distillation, obtains finished product sodium hydroxide solution.
Another aspect provides a kind of method improving concentration of sodium hydroxide solution and purity.Said method comprising the steps of: in pending sodium hydroxide solution, add alcohol sodium compound, the water generation hydrolysis reaction in described alcohol sodium compound and pending sodium hydroxide solution generates Organic Alcohol and sodium hydroxide; After question response is complete, filters and remove insoluble impurity, Organic Alcohol is removed in distillation, obtains finished product sodium hydroxide solution.
In one exemplary embodiment, described alcohol sodium compound is sodium ethylate and/or sodium tert-butoxide.
In one exemplary embodiment, when described alcohol sodium compound is sodium ethylate, the temperature of distillation is more than 79 DEG C.
In one exemplary embodiment, described alcohol sodium compound be sodium tert-butoxide or the mixture of sodium tert-butoxide and sodium ethylate time, the temperature of distillation is more than 83 DEG C.
In one exemplary embodiment, the mol ratio needing the water removed in described alcohol sodium compound in sodium element and sodium hydroxide solution is 1:1, or is calculated as follows:
Wherein,
for sodium ion quality in pending sodium hydroxide solution, unit is g; m
solutionfor the total mass of pending sodium hydroxide solution, unit is g; X is the mole number of the alcohol sodium compound added, and unit is mol;
for the mass concentration of sodium ion in finished product sodium hydroxide solution, unit is g/Kg.
In one exemplary embodiment, described method stirs while being also included in described hydrolysis reaction.
Compared with prior art, beneficial effect of the present invention comprises: in pending sodium hydroxide solution, add alcohol sodium compound by adding, utilize its hydrolysis properties, generate sodium hydroxide and alcohol, compared with common distillation, by the method for this invention, efficiently can remove unnecessary water from aqueous sodium hydroxide solution, greatly save the time, and mention the concentration of sodium hydroxide, remove a part of impurity simultaneously, make the sustainable recycle of sodium hydroxide, supplementing of sodium hydroxide is reduced in working cycle, shorten the production cycle, reduce energy consumption and equipment loss, application prospect is good.
Embodiment
Hereinafter, the method according to raising naoh concentration of the present invention will be described in detail in conjunction with exemplary embodiment.
For the sodium hydroxide solution produced in Industrial processes, its concentration is low and containing some foreign ions, in order to can recycling, needs to improve concentration of sodium hydroxide solution and purity.Such as, sodium hydroxide sub-molten salt leaches valuable metal element in metallic ore and remaining sodium hydroxide solution after removing (such as extracting in the basic conditions) part valuable metal element, or remaining sodium hydroxide solution through water logging leaching valuable metal element and after removing part valuable metal element after sodium hydrate solid and slag or ore deposit roasting, wherein carry foreign ion (such as, SO
4 2-, Cl
-, SiO
3 2-, PO
4 3-deng), certainly, the sodium hydroxide solution that the present invention can process is not limited thereto, and can also be the sodium hydroxide solution produced in other techniques.
The method of concentration of sodium hydroxide solution and purity is improved according to the present invention, comprise the following steps: in pending sodium hydroxide solution, add alcohol sodium compound, wherein, alcohol sodium compound refers to the compound that the hydrogen of hydroxyl in alcohol molecule is replaced by sodium Metal 99.5, and the water generation hydrolysis reaction in described alcohol sodium compound and pending sodium hydroxide solution generates Organic Alcohol and sodium hydroxide; After question response is complete, filters and remove insoluble impurity, Organic Alcohol is removed in distillation, obtains finished product sodium hydroxide solution.
The method by adding a certain amount of alcohol sodium compound in sodium hydroxide solution, utilize alcohol sodium compound and water to react and generate Organic Alcohol and sodium hydroxide, can utilize that sodium hydroxide and Organic Alcohol dissolve each other and some impurity are insoluble to Organic Alcohol simultaneously, and because the water in sodium hydroxide solution reduces, namely the solvent of dissolved impurity tails off, change impurity equilibrium system, partial impurities is separated out, thus the insoluble impurity of a removed by filtration part, then distill, make the Organic Alcohol gasification in filtrate for steam and collect with using it for anything else or selling through condensation, and the solution of remainder is the highly purified sodium hydroxide solution of high density.
Wherein, described alcohol sodium compound can adopt sodium ethylate and/or sodium tert-butoxide.When the alcohol sodium compound added is sodium ethylate, the temperature of distillation is more than 79 DEG C.When the alcohol sodium compound added be sodium tert-butoxide or the mixture of sodium tert-butoxide and sodium ethylate time, the temperature of distillation is more than 83 DEG C.Method of the present invention can process the sodium hydroxide solution of any water content, and the consumption of alcohol sodium compound can be determined according to following two kinds of modes, the water that the first is removed according to the needs in pending sodium hydroxide solution is determined, namely needs the mol ratio of the water removed to be 1:1 in sodium element and sodium hydroxide solution in alcohol sodium compound; Or be calculated as follows:
In above formula,
for sodium ion quality in pending sodium hydroxide solution, unit is g; m
solutionfor the total mass of pending sodium hydroxide solution, unit is g; X is the mole number of the alcohol sodium compound added, and unit is mol;
for the mass concentration of sodium ion in finished product sodium hydroxide solution, unit is g/Kg.
Above two kinds of account forms can be selected arbitrarily, and wherein the former is applicable to the quality needing the water removed in known pending sodium hydroxide solution, and the latter is applicable to the concentration of sodium ion in known pending sodium hydroxide solution.
Further, can also stir while described hydrolysis reaction.
In one exemplary embodiment, the method improving concentration of sodium hydroxide solution and purity comprises the following steps:
A. in pending sodium hydroxide solution, add alcohol sodium compound, and limit edged stirs.
B. after not producing bubble, 3 ~ 5min stops stirring, and filters to remove partial impurities, obtains filtrate.
C. distill filtrate to constant weight, obtain finished product sodium hydroxide solution.Wherein, be sodium ethylate when what add in step a, then under the temperature condition of 79 DEG C, be evaporated to constant weight; Be sodium tert-butoxide or sodium tert-butoxide and sodium ethylate mixture when what add in step a, then under the condition of 83 DEG C, be evaporated to constant weight.
D. retort solution is collected.
It should be noted that, when pending sodium hydroxide solution moderate purity high density is low, when namely only needing improve concentration and do not need removal of impurities process, the method of the raising concentration of sodium hydroxide solution provided according to a further aspect in the invention can be provided, the method is compared with the method for purity with the above-mentioned concentration of sodium hydroxide solution that improves simultaneously, except eliminating the removal step before the complete distilation steps afterwards of described hydrolysis reaction, all the other steps are consistent.
In order to understand above-mentioned exemplary embodiment of the present invention better, below in conjunction with concrete example, it is further described.
Example 1
(Na ion concentration is 80.00g/Kg, SO to get 1000g sodium hydroxide solution
4 2-for 5g/Kg, Cl
-for 0.86g/Kg, SiO
3 2-for 1.86g/Kg, PO
4 3-for 0.06g/Kg), add sodium ethylate 2.67mol, dropping limit, limit is stirred, after not producing bubble, stir 3min again, filter out some throw outs, then concentrated distillation, distillation temperature is 79 DEG C, distillation time is 0.5h, and collect ethanol 93g, in remaining sodium hydroxide solution, na concn is 133.33g/Kg, SO
4 2-for 2g/Kg, Cl
-for 0.46g/Kg, SiO
3 2-for 0.86g/Kg, PO
4 3-for 0.03g/Kg.
Example 2
(Na ion concentration is 80.00g/Kg, SO to get the sodium hydroxide solution of 1000g
4 2-for 5g/Kg, Cl
-for 0.86g/Kg, SiO
3 2-for 1.86g/Kg, PO
4 3-for 0.06g/Kg), add sodium tert-butoxide 2.67mol, dropping limit, limit is stirred, and after not producing bubble, then stirs 5min, filters out some throw outs, then concentrated distillation, and distillation temperature is 83 DEG C, and distillation time is 0.8h, collects trimethyl carbinol 197g.In remaining sodium hydroxide solution, Na ion concentration is 133.33g/Kg, SO
4 2-for 2.03g/Kg, Cl
-for 0.45g/Kg, SiO
3 2-for 0.87g/Kg, PO
4 3-for 0.04g/Kg.
Example 3
(Na ion concentration is 100.00g/Kg, SO to get 5000g sodium hydroxide solution
4 2-for 5g/Kg, Cl
-for 0.86g/Kg, SiO
3 2-for 1.86g/Kg, PO
4 3-for 0.06g/Kg), add sodium ethylate 1.236mol, dropping limit, limit is stirred, and after not producing bubble, then stirs 3min, filters out some throw outs, then concentrated distillation, and distillation temperature is 79 DEG C, and distillation time is 0.6h, collects ethanol 56.8g.In remaining sodium hydroxide solution, Na ion concentration is 125g/Kg, SO
4 2-for 3.04g/Kg, Cl
-for 0.55g/Kg, SiO
3 2-for 0.97g/Kg, PO
4 3-for 0.05g/Kg.
Example 4
(Na ion concentration is 100.00g/Kg, SO to get 5000g sodium hydroxide solution
4 2-for 5g/Kg, Cl
-for 0.86g/Kg, SiO
3 2-for 1.86g/Kg, PO
4 3-for 0.06g/Kg), add sodium tert-butoxide 1.236mol, dropping limit, limit is stirred, and after not producing bubble, then stirs 4min, filters out some throw outs, then concentrated distillation, and distillation temperature is 83 DEG C, and distillation time is 1h, collects trimethyl carbinol 91.6g.In remaining sodium hydroxide solution, Na ion concentration is 125g/Kg, SO
4 2-for 3.14g/Kg, Cl
-for 0.53g/Kg, SiO
3 2-for 0.99g/Kg, PO
4 3-for 0.05g/Kg.
Example 5
(Na ion concentration is 100.00g/Kg, SO to get 5000g sodium hydroxide solution
4 2-for 5g/Kg, Cl
-for 0.86g/Kg, SiO
3 2-for 1.86g/Kg, PO
4 3-for 0.06g/Kg), add sodium ethylate 0.8mol, sodium tert-butoxide 0.4236mol, dropping limit, limit is stirred, after not producing bubble, then stir 5min, filter out some throw outs, then concentrated distillation, distillation temperature is 83 DEG C, and distillation time is 0.75h, collects mixing retort solution 67.9g.In remaining sodium hydroxide solution, Na ion concentration is 125g/Kg, SO
4 2-for 3.08g/Kg, Cl
-for 0.54g/Kg, SiO
3 2-for 0.98g/Kg, PO
4 3-for 0.05g/Kg.
Comparative example 1
(Na ion concentration is 80.00g/Kg, SO to get 1000g sodium hydroxide solution
4 2-for 5g/Kg, Cl
-for 0.86g/Kg, SiO
3 2-for 1.86g/Kg, PO
4 3-for 0.06g/Kg), adopt concentrated distillation, distillation temperature is 100 DEG C, and distillation time is 2.5h, and collect distilled water 400g, in remaining sodium hydroxide solution, Na ion concentration is 133.33g/Kg, SO
4 2-for 8.33g/Kg, Cl
-for 1.43g/Kg, SiO
3 2-for 3.1g/Kg, PO
4 3-for 0.1g/Kg.
Comparative example 2
(Na ion concentration is 100.00g/Kg, SO to get 5000g sodium hydroxide solution
4 2-for 5g/Kg, Cl
-for 0.86g/Kg, SiO
3 2-for 1.86g/Kg, PO
4 3-for 0.06g/Kg), adopt concentrated distillation, distillation temperature is 100 DEG C, and distillation time is 3.5h, collects distilled water 1000g.In remaining sodium hydroxide solution, Na ion concentration is 125g/Kg, SO
4 2-for 6.25g/Kg, Cl
-for 1.07g/Kg, SiO
3 2-for 2.32g/Kg, PO
4 3-for 0.07g/Kg.
Can find out, method of the present invention can improve naoh concentration and remove partial impurities, compared with straight run distillation of the prior art, has greatly saved the time, has been conducive to the recycle and reuse of sodium hydroxide.
Although above by describing the present invention in conjunction with exemplary embodiment, it will be apparent to those skilled in the art that when not departing from the spirit and scope that claim limits, various amendment and change can be carried out to exemplary embodiment of the present invention.
Claims (7)
1. improve a method for concentration of sodium hydroxide solution, it is characterized in that, pending sodium hydroxide solution purity high density is low, and described method does not need removal of impurities for improving the concentration of pending sodium hydroxide solution, said method comprising the steps of:
In pending sodium hydroxide solution, add alcohol sodium compound, the water generation hydrolysis reaction in described alcohol sodium compound and pending sodium hydroxide solution generates Organic Alcohol and sodium hydroxide;
After question response is complete, Organic Alcohol is removed in distillation, obtains finished product sodium hydroxide solution.
2. improve a method for concentration of sodium hydroxide solution and purity, it is characterized in that, said method comprising the steps of:
In pending sodium hydroxide solution, add alcohol sodium compound, the water generation hydrolysis reaction in described alcohol sodium compound and pending sodium hydroxide solution generates Organic Alcohol and sodium hydroxide, and sodium hydroxide and Organic Alcohol dissolve each other and some impurity are insoluble to Organic Alcohol;
After question response is complete, the water in sodium hydroxide solution reduces, and the solvent of dissolved impurity tails off, and partial impurities is separated out, and filters and removes insoluble impurity, distills and removes Organic Alcohol, obtain finished product sodium hydroxide solution.
3. method according to claim 1 and 2, is characterized in that, described alcohol sodium compound is sodium ethylate and/or sodium tert-butoxide.
4. method according to claim 3, is characterized in that, when described alcohol sodium compound is sodium ethylate, the temperature of distillation is more than 79 DEG C.
5. method according to claim 3, is characterized in that, when described alcohol sodium compound is the mixture of sodium tert-butoxide or sodium tert-butoxide and sodium ethylate, the temperature of distillation is more than 83 DEG C.
6. method according to claim 1 and 2, is characterized in that, the mol ratio needing the water removed in described alcohol sodium compound in sodium element and sodium hydroxide solution is 1:1, or is calculated as follows:
Wherein,
sodium ion quality in pending sodium hydroxide solution, unit is g; m
solutionfor the total mass of pending sodium hydroxide solution, unit is g; X is the mole number of the alcohol sodium compound added, and unit is mol;
for the mass concentration of sodium ion in finished product sodium hydroxide solution, unit is g/kg.
7. method according to claim 1 and 2, is characterized in that, described method stirs while being also included in described hydrolysis reaction.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101077981A (en) * | 2006-05-24 | 2007-11-28 | 宁波中一石化科技有限公司 | Method for regenerating alkali liquor containing sodium thioalcohol |
| CN101148280A (en) * | 2007-09-05 | 2008-03-26 | 三达膜科技（厦门）有限公司 | Purifying and reclaiming method for alkali waste water based on film technique |
| CN101371967A (en) * | 2007-08-24 | 2009-02-25 | 宁波中一石化科技有限公司 | Liquid gas sweetening alkali liquor oxidized regeneration method and apparatus |
| CN101962566A (en) * | 2009-07-21 | 2011-02-02 | 宁波中一石化科技有限公司 | Mercaptan removed alkali liquid oxidation regeneration method and device thereof |
-
2013
- 2013-09-30 CN CN201310459578.9A patent/CN103496718B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101077981A (en) * | 2006-05-24 | 2007-11-28 | 宁波中一石化科技有限公司 | Method for regenerating alkali liquor containing sodium thioalcohol |
| CN101371967A (en) * | 2007-08-24 | 2009-02-25 | 宁波中一石化科技有限公司 | Liquid gas sweetening alkali liquor oxidized regeneration method and apparatus |
| CN101148280A (en) * | 2007-09-05 | 2008-03-26 | 三达膜科技（厦门）有限公司 | Purifying and reclaiming method for alkali waste water based on film technique |
| CN101962566A (en) * | 2009-07-21 | 2011-02-02 | 宁波中一石化科技有限公司 | Mercaptan removed alkali liquid oxidation regeneration method and device thereof |
Non-Patent Citations (1)
| Title |
|---|
| 吴鸣声.《有机化学基本实验》.《有机化学基本实验》.江西人民出版社,1980,(第1版),第55-56页. * |
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