CN104477946A - Purification method of industrial-grade sodium carbonate - Google Patents
Purification method of industrial-grade sodium carbonate Download PDFInfo
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- CN104477946A CN104477946A CN201410758432.9A CN201410758432A CN104477946A CN 104477946 A CN104477946 A CN 104477946A CN 201410758432 A CN201410758432 A CN 201410758432A CN 104477946 A CN104477946 A CN 104477946A
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- sodium carbonate
- anhydrous sodium
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Abstract
The invention discloses a purification method of industrial-grade sodium carbonate, which comprises the following steps: dissolving the raw material industrial anhydrous sodium carbonate in high-purity water, adding a polyaluminum hydroxychloride adsorbent, filtering through a cellulose acetate microfiltration membrane, crystallizing, melting and calcining to obtain the reagent-grade anhydrous sodium carbonate. The purity of the obtained anhydrous sodium carbonate is up to 99.9% (wt), the impurity anion content is respectively 10 ppm below, the impurity cation content is respectively 5 ppm below, and thus, the anhydrous sodium carbonate satisfies the top-grade purity standard for chemical reagent anhydrous sodium carbonate in GBT639-2008.
Description
Technical field:
The present invention relates to inorganic chemical product technical field of purification, is with technical grade sodium carbonate for raw material concretely, purifies, to produce the method for SILVER REAGENT anhydrous sodium carbonate, be applicable to the purge process of technical grade sodium carbonate to it.
Background technology:
China's technical grade sodium carbonate throughput has ranked world's first, as large inorganic chemical product, because the foreign matter content of technical grade sodium carbonate is higher, can not meet the service requirements of domestic and international electron trade, fine chemistry industry, teaching and field of scientific study.At present, the purification techniques comparatively backwardness of China's technical grade sodium carbonate, SILVER REAGENT sodium carbonate manufacturer scattered distribution, small scale, production technology, the seed output and quality of SILVER REAGENT sodium carbonate can not meet the market requirement.Along with the continuous expansion that sodium carbonate is applied at high-technology field, need the supply of a large amount of SILVER REAGENT sodium carbonate, more need the method for purification of comparatively advanced technical grade sodium carbonate to carry out technical support to reagent manufacturer.
In prior art, the purification process of technical grade sodium carbonate adopts chemical precipitation-crystallization process usually: take industrial sodium carbonate as raw material, make solution, carries out precipitation process to anions and canons, and by sodium carbonate solution crystallization, dewatering obtains the sodium carbonate of purifying.Preparation research (the Li Debo of high purity sodium carbonate, Han Shuxia etc., Shandong chemical industry, 37th volume the 6th phase in 2008) disclose a kind of method of mode prepared calcium carbonate sodium of precipitation, complexing, crystallization, but the method complex operation, so product purity is low, high expensive, the sulfide that precipitation process uses likely is reintroduced back to new impurity in sodium carbonate, there is complexing agent can not reusable problem, is difficult to obtain meeting the pure standard of chemical reagent anhydrous sodium carbonate GBT-639-2008 top grade.In addition, the purification process somebody of technical grade sodium carbonate adopts ion-exchange-crystallization process: be raw material with industrial sodium carbonate, and make solution, carry out adsorption treatment to negatively charged ion, by sodium carbonate solution crystallization, dewatering obtains the sodium carbonate of purifying.A kind of preparation method (Gu Hongjie of SILVER REAGENT anhydrous sodium carbonate, Chen Hong etc., Chinese patent application publication No. CN 103601220A, date of publication: 2014.02.26) disclose one ionic adsorption, millipore filtration, the method of the mode prepared calcium carbonate sodium of crystallization, but the method complicated operation, high expensive, the organic amine solid-carried catalyst that adsorption process uses can only remove impurity anions, impurity cationic is still stayed in sodium carbonate, organic amine solid-carried catalyst does not have commercialization, there is the problem that organic amine solid-carried catalyst is prepared oneself, also be difficult to reach and meet the pure standard of chemical reagent anhydrous sodium carbonate GBT639-2008 top grade.
Summary of the invention:
Problem to be solved by this invention is the method for purification providing a kind of technical grade sodium carbonate, and complicated to overcome prior art operating process, product purity is low, the deficiency of high expensive.
Technical thought of the present invention is as follows:
With industrial anhydrous sodium carbonate for raw material, be dissolved in high purity water, add poly-aluminium chlorohydroxide sorbent material, through cellulose acetate millipore filtration membrane filtration, crystallization, melting, calcining, obtains SILVER REAGENT anhydrous sodium carbonate.
Technical scheme of the present invention comprises the steps:
Industrial anhydrous sodium carbonate is added at normal temperatures specific impedance to be greater than in the high purity water of 18M Ω .cm and to dissolve, add poly-aluminium chlorohydroxide sorbent material, 40-50 DEG C is heated under stirring (0.5 hour), insulation leaves standstill 1-1.5 hour, filtered while hot removing colloid solid phase, acetyl cellulose micropore filtering film by aperture 0.1-0.22 μm under the filtrate insulation obtained carries out membrane filtration, and the filtrate obtained concentrates, and the concentrated ratio dewatered is 0.2-0.5.Crystallize out under the condition of 2-6 DEG C, carries out melting to this crystals of sodium carbonate, then under 80 DEG C of-90 DEG C of conditions, carries out recrystallization, leach recrystallization product, washed and filtered the solid that obtains afterwards at the temperature lower calcination of 280-330 DEG C, pulverize, obtain SILVER REAGENT anhydrous sodium carbonate.
According to the present invention, the industrial anhydrous sodium carbonate used meets the standard of GB210-92 salable product, the mass volume ratio of industrial anhydrous sodium carbonate and high purity water, 1: 3-5, g/ml, the mass ratio of industrial anhydrous sodium carbonate and poly-aluminium chlorohydroxide sorbent material is: 10: 1, g/g.
Poly-aluminium chlorohydroxide sorbent material used in the present invention commercialization, meets GB15892-2009 premium grads standard.
The feature of the poly-aluminium chlorohydroxide sorbent material that the present invention utilizes, poly-aluminium chlorohydroxide forms floss colloid in water, not only effectively to water-insoluble coagulation, and effectively can reduce Fe in solution
3+, Ca
2+, Cu
2+deng impurity cationic, this adsorbent amount is few, is easy to commercially buy.
The present invention, by carrying out melting to this crystals of sodium carbonate, can reduce Fe in solution further
3+, Ca
2+, Cu
2+deng impurity cationic, effectively reduce Cl in solution simultaneously
-, SO
4 2-, SiO
2-deng impurity cationic.By melting, occur to react as follows: Na
2cO
310H
2o=Na
2cO
32H
2o+2H
2o, NaCO
32H
2o=Na
2cO
3+ 2H
2o.By sloughing the crystal water in crystal sodium carbonate, making to be embedded in soluble impurity ion-transfer in crystal in water, soluble impurity ion can be removed further.
After testing, the purity of the SILVER REAGENT anhydrous sodium carbonate obtained by method of the present invention reaches 99.9wt%, wherein the content of impurity anions is at below 10ppm, and the content of impurity cationic, at below 5ppm, meets the pure standard of chemical reagent anhydrous sodium carbonate GB639-2008 top grade.
The present invention's advantageous effect compared with prior art:
1. poly-aluminium chlorohydroxide sorbent material used in the present invention effectively can remove impurity cationic, and this adsorbent amount is few, is easy to commercially buy.
2. the present invention is by carrying out melting to this crystals of sodium carbonate, can reduce Fe in solution further
3+, Ca
2+, Cu
2+deng impurity cationic, effectively reduce Cl in solution simultaneously
-, SO
4 2-, SiO
2-deng impurity cationic, this process operation is simple and easy to do, without the need to increasing unclassified stores.
3. method of purification of the present invention is easy and simple to handle, good impurity removing effect, and the anhydrous sodium carbonate constant product quality obtained, cost is lower, is very suitable for suitability for industrialized production.
Embodiment:
Below by specific embodiment, the present invention will be further described, but implement not limit the scope of the invention from example.
Embodiment 1
200g industry anhydrous sodium carbonate is dissolved at normal temperatures 600mL is greater than 18M Ω .cm high purity water than resistance, add 20g and gather aluminium chlorohydroxide sorbent material, 48 DEG C are heated under stirring (0.5 hour), insulation leaves standstill 1 hour, filtered while hot removing colloid solid phase, membrane filtration is carried out by the acetyl cellulose micropore filtering film in 0.22 μm, aperture under the filtrate insulation obtained, the filtrate obtained concentrates, after removing 120mL water, cool to 3 DEG C, crystallize out, melting is carried out to this crystals of sodium carbonate, then under 80 DEG C of conditions, recrystallization is carried out, leach recrystallization product, washed and filter the solid obtained afterwards and calcine in retort furnace at 280 DEG C of temperature, pulverize, obtain 160g SILVER REAGENT anhydrous sodium carbonate.
Embodiment 2
100g industry anhydrous sodium carbonate is dissolved at normal temperatures 500mL is greater than 18M Ω .cm high purity water than resistance, add 10g and gather aluminium chlorohydroxide sorbent material, 50 DEG C are heated under stirring (0.5 hour), insulation leaves standstill 1.5 hours, filtered while hot removing colloid solid phase, membrane filtration is carried out by the acetyl cellulose micropore filtering film in 0.1 μm, aperture under the filtrate insulation obtained, the filtrate obtained concentrates, after removing 250mL water, cool to 1 DEG C, crystallize out, melting is carried out to this crystals of sodium carbonate, then under 90 DEG C of conditions, recrystallization is carried out, leach recrystallization product, washed and filter the solid obtained afterwards and calcine in retort furnace at 300 DEG C of temperature, pulverize, obtain 80g SILVER REAGENT anhydrous sodium carbonate.
Embodiment 1-2 Product checking result is as follows:
| Test item | Standard value | Measured value 1 | Measured value 2 |
| Content (Na 2CO 3)，％ | ≥99.8 | 99.9 | 99.9 |
| Water-insoluble, % | ≤0.005 | 0.002 | 0.001 |
| Water-insoluble, % | ≤0.005 | 0.002 | 0.001 |
| Loss on ignition (300 DEG C), % | ≤0.5 | 0.2 | 0.1 |
| Muriate (Cl), ppm | ≤10 | 7 | 6 |
| Sulphur compound (SO 4 2+)，ppm | ≤30 | 8 | 7 |
| Total nitrogen (N), ppm | ≤10 | 7 | 6 |
| Phosphoric acid salt and silicate (SiO 3)，ppm | ≤25 | 7 | 8 |
| Magnesium (Mg), ppm | ≤5 | 3 | 2 |
| Aluminium (Al), ppm | ≤10 | 3 | 4 |
| Potassium (K), ppm | ≤50 | 3 | 4 |
| Calcium (Ca), ppm | ≤50 | 3 | 4 |
| Iron (Fe), ppm | ≤3 | 2 | 3 |
| Heavy metal (in Pb), ppm | ≤5 | 2 | 3 |
The anhydrous sodium carbonate obtained utilizing the present invention detects the instrument used: positively charged ion adopts plasma mass spectrometry (ICP-MS), and negatively charged ion adopts ionic liquid phase chromatographic instrument (IC), and moisture content adopts karl Fischer moisture content tester.
As seen from the above table, the purity of the anhydrous sodium carbonate that the present invention obtains reaches 99.9% (wt), wherein the content of impurity anions is all at below 10ppm, and the content of impurity cationic, all at below 5ppm, meets the pure standard of chemical reagent anhydrous sodium carbonate GBT639-2008 top grade.
Above embodiment is only in order to illustrate technical scheme of the present invention and on-fixed.Although illustrate invention has been with reference to fixing embodiment, the those skilled in the art of the industry are understood that, modify to the technical scheme of invention or replace on an equal basis, and not departing from the scope of technical solution of the present invention, it all should be included in right of the present invention.
Claims (5)
1. a method of purification for technical grade sodium carbonate, comprises the steps:
Industrial anhydrous sodium carbonate is added at normal temperatures specific impedance to be greater than in the high purity water of 18M Ω .cm and to dissolve, add poly-aluminium chlorohydroxide sorbent material, 40-50 DEG C is heated under stirring (0.5 hour), insulation leaves standstill 1-1.5 hour, filtered while hot removing colloid solid phase, acetyl cellulose micropore filtering film by aperture 0.1-0.22 μm under the filtrate insulation obtained carries out membrane filtration, and the filtrate obtained concentrates, and the concentrated ratio dewatered is 0.2-0.5.Crystallize out under the condition of 2-6 DEG C, carries out melting to this crystals of sodium carbonate, then under 80 DEG C of-90 DEG C of conditions, carries out recrystallization, leach recrystallization product, washed and filtered the solid that obtains afterwards at the temperature lower calcination of 280-330 DEG C, pulverize, obtain SILVER REAGENT anhydrous sodium carbonate.
2. the method for purification of a kind of technical grade sodium carbonate according to claim 1, is characterized in that, described industrial anhydrous sodium carbonate and the mass volume ratio of high purity water are 1: 3-5, g/ml.
3. the method for purification of a kind of technical grade sodium carbonate according to claim 1, is characterized in that, the mass ratio of described industrial anhydrous sodium carbonate and poly-aluminium chlorohydroxide sorbent material is: 10: 1, g/g.
4. the method for purification of the technical grade sodium carbonate according to claim 1-3 any one, is characterized in that, described technical grade sodium carbonate meets the standard of GB210-92 salable product.
5. the method for purification of a kind of technical grade sodium carbonate according to right 1, it is characterized in that, the filtrate obtained after membrane filtration concentrates, and the concentrated ratio dewatered is 0.2-0.5.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109110786A (en) * | 2017-06-22 | 2019-01-01 | 上海氯德新材料科技有限公司 | The method of micro-calcium is removed in sodium carbonate purification |
| CN110790288A (en) * | 2019-11-25 | 2020-02-14 | 天津渤化工程有限公司 | Electronic alkali production system and electronic alkali production method |
| CN115193293A (en) * | 2022-04-19 | 2022-10-18 | 湖南银桥食品添加剂有限公司 | Sodium bicarbonate production equipment and production method thereof |
Citations (3)
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|---|---|---|---|---|
| US4288419A (en) * | 1980-04-04 | 1981-09-08 | Intermountain Research & Develop. Corp. | Enhanced recovery of sodium carbonate from NaCl-containing sodium carbonate solutions |
| CN101700897A (en) * | 2009-12-08 | 2010-05-05 | 湖南尔康制药有限公司 | Pharmaceutical grade anhydrous sodium carbonate and preparation method thereof |
| CN103601220A (en) * | 2013-12-02 | 2014-02-26 | 国药集团化学试剂有限公司 | Preparation method for reagent-grade anhydrous sodium carbonate |
-
2014
- 2014-12-08 CN CN201410758432.9A patent/CN104477946B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4288419A (en) * | 1980-04-04 | 1981-09-08 | Intermountain Research & Develop. Corp. | Enhanced recovery of sodium carbonate from NaCl-containing sodium carbonate solutions |
| CN101700897A (en) * | 2009-12-08 | 2010-05-05 | 湖南尔康制药有限公司 | Pharmaceutical grade anhydrous sodium carbonate and preparation method thereof |
| CN103601220A (en) * | 2013-12-02 | 2014-02-26 | 国药集团化学试剂有限公司 | Preparation method for reagent-grade anhydrous sodium carbonate |
Non-Patent Citations (2)
| Title |
|---|
| 单金环等: "重结晶法提纯生产基准碳酸钠", 《中国材料科技与设备》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109110786A (en) * | 2017-06-22 | 2019-01-01 | 上海氯德新材料科技有限公司 | The method of micro-calcium is removed in sodium carbonate purification |
| CN109110786B (en) * | 2017-06-22 | 2020-11-10 | 上海氯德新材料科技有限公司 | Method for removing trace calcium in sodium carbonate refining |
| CN110790288A (en) * | 2019-11-25 | 2020-02-14 | 天津渤化工程有限公司 | Electronic alkali production system and electronic alkali production method |
| CN115193293A (en) * | 2022-04-19 | 2022-10-18 | 湖南银桥食品添加剂有限公司 | Sodium bicarbonate production equipment and production method thereof |
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