CN1082002A - A kind of method of POV sodium - Google Patents
A kind of method of POV sodium Download PDFInfo
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- CN1082002A CN1082002A CN 93111880 CN93111880A CN1082002A CN 1082002 A CN1082002 A CN 1082002A CN 93111880 CN93111880 CN 93111880 CN 93111880 A CN93111880 A CN 93111880A CN 1082002 A CN1082002 A CN 1082002A
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- sodium
- pov
- soda ash
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/16—Purification
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Abstract
The invention provides a kind of method of POV sodium, sodium sulfate prepared in reaction yellow soda ash after at first using bicarbonate of ammonia and making with extra care, in sodium carbonate solution, add a small amount of calcium hydroxide then, make the mixed alkali liquor that contains sodium hydroxide and yellow soda ash, react as precipitation agent and raw material sulphuric acid sodium with mixed alkali liquor again, remove wherein calcium and magnesium, after regulating pH, concentrate, filtration, drying make solid POV sodium.This method makes full use of this enterprise product sodium sulfate and the reaction of inexpensive bicarbonate of ammonia and makes mixed alkali liquor and make with extra care, and reduces production costs greatly, compares with direct making with extra care with soda ash and caustic soda, can reduce materials cost 40%.
Description
The present invention relates to a kind of material method of purification, particularly relate to a kind of method of POV sodium.
Be that raw material production sodium sulfate all adopts soda ash and the refining thick sodium sulfate liquid of caustic soda at present with the glauberite, remove wherein calcium and magnesium.But soda ash and caustic soda are in short supply, and the valency height, and production cost is increased.Chinese patent publication number 1069709 discloses a kind of novel method of refining sodium sulphate, be to react in glauberite, water and the lime adding ball mill (or bath) as scavenging agent, after leaching, filtration, make the coarse sulfide water that contains caustic soda, and then with the reaction of another kind of scavenging agent carbon ammonium, after filtering smart glass gall.The shortcoming of this method is, one because calcium hydroxide is slightly soluble in water (1.3 grams per liter water), generates Mg(OH with Mg++ reaction in the solution) 2 precipitations, remove the weak effect of magnesium; Amount of sodium hydroxide with sodium sulfate reaction generation is few simultaneously.They are two years old, because the amount with bicarbonate of ammonia reaction generation yellow soda ash is also few less for amount of sodium hydroxide, can not remove a large amount of calcium contained in the glauberite, they are three years old, when reacting in the coarse sulfide water that contains caustic soda with the adding of carbon ammonium, except that generating the yellow soda ash, also can generate sodium bicarbonate and ammonium sulfate simultaneously, and the existence of ammonium sulfate is unfavorable for that precipitation of calcium carbonate is complete with the sodium sulfate reaction with the sodium hydroxide reaction.
The object of the present invention is to provide a kind of is that raw material and sodium sulfate reaction make the mixed alkali liquor that contains sodium hydroxide and yellow soda ash with inexpensive bicarbonate of ammonia, uses the method for its POV sodium again.
The method of POV sodium of the present invention is.With the glauberite is initial feed, and its major ingredient is (by weight) sodium sulfate 32-39%, calcium sulfate 40-45%, sodium-chlor 0.3-0.4%, water-insoluble 10-13%, sal epsom 0.01-0.015%.Obtain the raw material sulphuric acid sodium solution after removing insolubles impurity.Its process for refining process is as follows, at first water, finished product sodium sulfate are added in the reactor, make its concentration generally be controlled at 35～55%(weight), in every liter of metabisulfite solution, add bicarbonate of ammonia 400～600 grams again, react 30～60 ℃ of temperature ranges, crossing filter cake is sodium bicarbonate, the main sulfur acid ammonium of filtrate and a small amount of sodium sulfate and bicarbonate of ammonia, and its chemical equation is:
Then sodium bicarbonate is put into reactor, and controlling concn is 18～20%(weight), carry out decomposition reaction in 130～150 ℃ and generate yellow soda ash, and the ratio that restrains calcium hydroxide in every liter of yellow soda ash adding 13-18 feeds intake, in 80-110 ℃ of temperature range, react, crossing filter cake is lime carbonate, and filtrate is sodium hydroxide and yellow soda ash mixed alkali liquor.Its chemical equation is:
Mixed alkali liquor with raw material sulphuric acid sodium solution and sodium hydroxide and yellow soda ash reacts at last, remove by filter wherein lime carbonate and magnesium hydroxide, obtain the POV sodium solution, control metabisulfite solution concentration is 18～22%(weight during reaction), can add 20-25 gram mixed alkali liquor in general every liter of raw material sulphuric acid sodium solution, 45～65 ℃ of temperature of reaction, its chemical equation is:
Owing in above-mentioned treating process, added excessive alkali lye so that remove calcium sulfate and sal epsom as far as possible completely, the pH value that makes its gained POV sodium solution is 9.5～10, the pH value is higher, needing adding ammonium sulfate to regulate its pH is 6-8, and this moment, used ammonium sulfate can adopt the reaction product of this technical process the first step.Its chemical equation is:
To adjust again that POV sodium solution after the pH value concentrates, filters, drying, make solid POV sodium.
The invention has the advantages that to make full use of enterprise product sodium sulfate and bicarbonate of ammonia reaction generation soda ash and caustic soda mixed alkali liquor, change original soda ash and the process of caustic soda of directly adopting, reduce product cost greatly, the expense that can economize in raw materials about 40%.
Describe the embodiment of the invention in detail below in conjunction with accompanying drawing.
Fig. 1: process flow diagram of the present invention.
Embodiment 1: 1000 premium on currency are put into reactor 1, add 500 and do gram POV sodium, 600 kilograms of bicarbonate of ammonia, stir, heat, reacted 50 minutes to 45 ± 2 ℃, after the filtration precipitate sodium bicarbonate is put into reactor 2 for 220 kilograms, add 1000 liters of stirrings of water, heat, reacted 40 minutes to 140 ± 5 ℃, add 15 kg of hydrogen calcium oxide then, stir, heat to 100 ± 5 ℃, reaction must contain the mixed alkali liquor of yellow soda ash and sodium hydroxide in 30 minutes.Put into mixing reactor after again raw material sulphuric acid sodium being mixed with the concentration of 200 grams per liters, and in 1 liter of metabisulfite solution: the ratios of 23 gram mixed alkali liquors add mixed alkali liquor, under 55 ± 2 ℃ of temperature, react, get the POV sodium solution after the filtration, and to adjust its pH value with ammoniumsulphate soln be 7.3, through concentrating, making solid POV sodium after the filtration, drying.Its product quality indicator is as shown in table 1.
Embodiment 2: 1000 premium on currency are put into reactor 1 add 550 gram product sodium sulfate, 600 gram bicarbonate of ammonia, stir, heat to 50 ± 5 ℃ of reactions 40 minutes, after the filtration precipitate sodium bicarbonate is put into reactor 2 for 250 kilograms, add 1000 liters of stirrings of water and heat to 145 ± 5 ℃, reacted 30 minutes, add 20 kg of hydrogen calcium oxide then, stir and heat, promptly get the mixed alkali liquor that contains yellow soda ash and sodium hydroxide after the filtration to 105 ± 5 ℃ of reactions 20 minutes.Raw material sulphuric acid sodium is formulated as 210 grams per liter concentration, in 1 liter of raw material sulphuric acid sodium: the ratios of 25 gram mixed alkali liquors add in the mixing tank, heat to 60 ± 5 ℃ and react, get the POV sodium solution after the filtration, and to adjust its pH value with ammoniumsulphate soln be 7, through concentrate, after the filtration, drying solid phase prod sodium sulfate.Its quality index is as shown in table 1.
Table 1: solid POV sodium quality index
| Standard GB 6009-85 | |
Embodiment 2 | |
| Sodium sulfate (%) | ≥99 | 99.3 | 99.2 |
| Calcium magnesium (in Mg%) | ≤0.35 | 0.23 | 0.21 |
| Sodium-chlor (in Cl%) | ≤0.35 | 0.11 | 0.21 |
| Water-insoluble (%) | ≤0.05 | 0.031 | 0.029 |
| Iron (in Fe%) | ≤0.002 | 0.0012 | 0.0013 |
| Moisture (%) | ≤0.2 | 0.13 | 0.15 |
| Whiteness | ≥80 | 87 | 85 |
| pH | 6-8 | 7.3 | 7 |
Claims (3)
1, a kind of method of POV sodium is characterized in that:
1) with bicarbonate of ammonia and sodium sulfate prepared in reaction yellow soda ash.
2) in yellow soda ash, add the mixed alkali liquor that calcium hydroxide obtains containing sodium hydroxide and yellow soda ash.
3) purify raw material sulphuric acid sodium with mixed alkali liquor, remove wherein calcium and magnesium, get the POV sodium solution.
4) regulating POV sodium solution pH with ammonium sulfate is 6-8, through concentrating, makes solid sodium sulfate after filtration, the drying.
2, the method for POV sodium as claimed in claim 1 is characterized in that the ratio of components of bicarbonate of ammonia and sodium sulfate reaction is 1 liter of metabisulfite solution: 400～600 gram sodium bicarbonates, wherein controlling metabisulfite solution concentration is 35-55%(weight).
3, the method for POV sodium as claimed in claim 1, the ratio of components that it is characterized in that yellow soda ash and calcium hydroxide reaction are 1 liter of sodium carbonate solution: 13～18 gram calcium hydroxides, the concentration of wherein controlling sodium carbonate solution is 11-13%(weight).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93111880 CN1082002A (en) | 1993-07-02 | 1993-07-02 | A kind of method of POV sodium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93111880 CN1082002A (en) | 1993-07-02 | 1993-07-02 | A kind of method of POV sodium |
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| Publication Number | Publication Date |
|---|---|
| CN1082002A true CN1082002A (en) | 1994-02-16 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 93111880 Pending CN1082002A (en) | 1993-07-02 | 1993-07-02 | A kind of method of POV sodium |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101844780A (en) * | 2010-05-20 | 2010-09-29 | 四川省川眉芒硝有限责任公司 | Process for treating mirabilite liquid |
| CN101602514B (en) * | 2008-06-10 | 2010-09-29 | 四川川眉特种芒硝有限公司 | Method for preparing special mirabilite with high purity |
| CN101837994B (en) * | 2009-03-20 | 2012-01-11 | 四川省川眉芒硝有限责任公司 | Production process of medicinal mirabilite |
| CN106865571A (en) * | 2017-03-20 | 2017-06-20 | 科莱环境工程（北京）有限公司 | A kind of method that chemical industry strong brine produces sodium bicarbonate and ammonium sulfate |
-
1993
- 1993-07-02 CN CN 93111880 patent/CN1082002A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101602514B (en) * | 2008-06-10 | 2010-09-29 | 四川川眉特种芒硝有限公司 | Method for preparing special mirabilite with high purity |
| CN101837994B (en) * | 2009-03-20 | 2012-01-11 | 四川省川眉芒硝有限责任公司 | Production process of medicinal mirabilite |
| CN101844780A (en) * | 2010-05-20 | 2010-09-29 | 四川省川眉芒硝有限责任公司 | Process for treating mirabilite liquid |
| CN106865571A (en) * | 2017-03-20 | 2017-06-20 | 科莱环境工程（北京）有限公司 | A kind of method that chemical industry strong brine produces sodium bicarbonate and ammonium sulfate |
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| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |