CN104477946B - A kind of method of purification of technical grade sodium carbonate - Google Patents
A kind of method of purification of technical grade sodium carbonate Download PDFInfo
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- CN104477946B CN104477946B CN201410758432.9A CN201410758432A CN104477946B CN 104477946 B CN104477946 B CN 104477946B CN 201410758432 A CN201410758432 A CN 201410758432A CN 104477946 B CN104477946 B CN 104477946B
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- sodium carbonate
- natrium carbonicum
- carbonicum calcinatum
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Abstract
The invention discloses the method for purification of a kind of technical grade sodium carbonate, with industry natrium carbonicum calcinatum for raw material, be dissolved in high purity water, add polyaluminium hydroxychloride adsorbent, through cellulose acetate microporous filter membrane filtration, crystallization, melted, calcining, obtain SILVER REAGENT natrium carbonicum calcinatum。The purity of the natrium carbonicum calcinatum that the present invention obtains reaches 99.9% (wt), and wherein the content of impurity anions is all at below 10ppm, and the content of impurity cationic, all at below 5ppm, meets the chemical reagent natrium carbonicum calcinatum pure standard of GBT639-2008 top grade。
Description
Technical field:
The present invention relates to inorganic chemical product technical field of purification, be with technical grade sodium carbonate for raw material concretely, it is purified, with the method producing SILVER REAGENT natrium carbonicum calcinatum, it is adaptable to the purge process of technical grade sodium carbonate。
Background technology:
China's technical grade sodium carbonate production capacity has ranked world's first, as large inorganic chemical product, owing to the impurity content of technical grade sodium carbonate is higher, it is impossible to meet the instructions for use of domestic and international electron trade, fine chemistry industry, teaching and field of scientific study。At present, the purification technique of China's technical grade sodium carbonate is comparatively backward, and SILVER REAGENT sodium carbonate manufacturer scattered distribution, small scale, the production technology of SILVER REAGENT sodium carbonate, yield and quality can not meet the market demand。Along with the continuous extension that sodium carbonate is applied at high-technology field, it is necessary to the supply of a large amount of SILVER REAGENT sodium carbonate, reagent manufacturer is carried out technical support by the method for purification with greater need for relatively advanced technical grade sodium carbonate。
In prior art, the purification process of technical grade sodium carbonate generally adopts chemical precipitation-crystallization process: with industrial sodium carbonate for raw material, make solution, and anions and canons is carried out precipitation process, and by sodium carbonate liquor crystallization, dewatering obtains the sodium carbonate of purification。Preparation research (the Li Debo of high-purity sodium carbonate, Han Shuxia etc., Shandong chemical industry, 37th volume the 6th phase in 2008) method that discloses the mode prepared calcium carbonate sodium of a kind of precipitation, complexation, 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 chelating agent can not reusable problem, it is difficult to obtain meeting the standard that chemical reagent natrium carbonicum calcinatum GBT-639-2008 top grade is pure。It addition, the purification process somebody of technical grade sodium carbonate adopts ion exchange-crystallization process: with industrial sodium carbonate for raw material, make solution, anion is carried out adsorption treatment, by sodium carbonate liquor crystallization, dewatering obtains the sodium carbonate of purification。A kind of preparation method (Gu Hongjie of SILVER REAGENT natrium carbonicum calcinatum, Chen Hong etc., Chinese patent application publication No. CN103601220A, date of publication: 2014.02.26) disclose one ionic adsorption, microporous filter, 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 still remains 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 it is difficult to reach to meet the chemical reagent natrium carbonicum calcinatum pure standard of GBT639-2008 top grade。
Summary of the invention:
To be solved by this invention haveing a problem in that the method for purification providing a kind of technical grade sodium carbonate, to overcome prior art operation process complicated, product purity is low, the deficiency of high expensive。
The technical thought of the present invention is as follows:
With industry natrium carbonicum calcinatum for raw material, it is dissolved in high purity water, adds polyaluminium hydroxychloride adsorbent, through cellulose acetate microporous filter membrane filtration, crystallization, melt, calcining, obtain SILVER REAGENT natrium carbonicum calcinatum。
Technical scheme comprises the steps:
Industry natrium carbonicum calcinatum is added in the specific impedance high purity water more than 18M Ω .cm at normal temperatures and dissolves, add polyaluminium hydroxychloride adsorbent, it is heated to 40-50 DEG C under stirring (0.5 hour), insulation stands 1-1.5 hour, filtered while hot removes colloid solid phase, carrying out membrane filtration by the acetyl cellulose micropore filtering film in 0.1-0.22 μm of aperture under the filtrate insulation obtained, the filtrate obtained concentrates, and the ratio that concentration dewaters is 0.2-0.5。Precipitate out crystal when 2-6 DEG C, this crystals of sodium carbonate is melted, under 80 DEG C of-90 DEG C of conditions, then carries out recrystallization, leach recrystallization product, the solid being filtrated to get after being washed, at the temperature lower calcination of 280-330 DEG C, is pulverized, is obtained SILVER REAGENT natrium carbonicum calcinatum。
According to the present invention, the industrial natrium carbonicum calcinatum used meets the standard of GB210-92 certified products, the mass volume ratio of industry natrium carbonicum calcinatum and high purity water, 1: 3-5, g/ml, the mass ratio of industry natrium carbonicum calcinatum and polyaluminium hydroxychloride adsorbent is: 10: 1, g/g。
Polyaluminium hydroxychloride adsorbent commercialization used in the present invention, meets GB15892-2009 high-class product standard。
The feature of the polyaluminium hydroxychloride adsorbent that the present invention utilizes, polyaluminium hydroxychloride forms floccule colloid in water, not only effectively to water-insoluble coagulation, and can effectively reduce Fe in solution3+、Ca2+、Cu2+Deng impurity cationic, this adsorbent amount is few, it is easy to commercially buy。
The present invention, by this crystals of sodium carbonate is melted, can reduce Fe in solution further3+、Ca2+、Cu2+Deng impurity cationic, effectively reduce Cl in solution simultaneously-、SO4 2-、SiO2-Deng impurity cationic。By melted, there is following reaction: Na2CO3·10H2O=Na2CO3·2H2O+2H2O, NaCO3·2H2O=Na2CO3+2H2O。By sloughing the water of crystallization in crystal sodium carbonate, make the soluble impurity ion-transfer being embedded in crystal in water, it is possible to remove soluble impurity ion further。
After testing, the purity of the SILVER REAGENT natrium carbonicum calcinatum obtained by the method for 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 chemical reagent natrium carbonicum calcinatum pure standard of GB639-2008 top grade。
Present invention advantageous effect compared with prior art:
1. polyaluminium hydroxychloride adsorbent used in the present invention can effectively remove impurity cationic, and this adsorbent amount is few, it is easy to commercially buy。
2. the present invention is by melting this crystals of sodium carbonate, can reduce Fe in solution further3+、Ca2+、Cu2+Deng impurity cationic, effectively reduce Cl in solution simultaneously-、SO4 2-、SiO2-Deng impurity cationic, this process operation is simple and easy to do, it is not necessary to increase unclassified stores。
3. the method for purification of the present invention is easy and simple to handle, good impurity removing effect, the natrium carbonicum calcinatum constant product quality obtained, less costly, is extremely suitable for industrial production。
Detailed description of the invention:
Below by specific embodiment, the present invention will be further described, but implements to be not limiting as protection scope of the present invention from example。
Embodiment 1
200g industry natrium carbonicum calcinatum is dissolved at normal temperatures 600mL than the resistance high purity water more than 18M Ω .cm, add 20g polyaluminium hydroxychloride adsorbent, it is heated to 48 DEG C under stirring (0.5 hour), insulation stands 1 hour, filtered while hot removes colloid solid phase, membrane filtration is carried out by the acetyl cellulose micropore filtering film in 0.22 μm of aperture under the filtrate insulation obtained, the filtrate obtained concentrates, after removing 120mL water, cool to 3 DEG C, precipitate out crystal, this crystals of sodium carbonate is melted, then under 80 DEG C of conditions, carry out recrystallization, leach recrystallization product, the solid being filtrated to get after being washed is calcined in Muffle furnace at 280 DEG C of temperature, pulverize, obtain 160g SILVER REAGENT natrium carbonicum calcinatum。
Embodiment 2
100g industry natrium carbonicum calcinatum is dissolved at normal temperatures 500mL than the resistance high purity water more than 18M Ω .cm, add 10g polyaluminium hydroxychloride adsorbent, it is heated to 50 DEG C under stirring (0.5 hour), insulation stands 1.5 hours, filtered while hot removes colloid solid phase, membrane filtration is carried out by the acetyl cellulose micropore filtering film in 0.1 μm of aperture under the filtrate insulation obtained, the filtrate obtained concentrates, after removing 250mL water, cool to 1 DEG C, precipitate out crystal, this crystals of sodium carbonate is melted, then under 90 DEG C of conditions, carry out recrystallization, leach recrystallization product, the solid being filtrated to get after being washed is calcined in Muffle furnace at 300 DEG C of temperature, pulverize, obtain 80g SILVER REAGENT natrium carbonicum calcinatum。
Embodiment 1-2 Product checking result is as follows:
| Detection project | Standard value | Measured value 1 | Measured value 2 |
| Content (Na2CO3), % | ≥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 |
| Chloride (Cl), ppm | ≤10 | 7 | 6 |
| Sulphur compound (SO4 2+), ppm | ≤30 | 8 | 7 |
| Total nitrogen (N), ppm | ≤10 | 7 | 6 |
| Phosphate and silicate (SiO3), ppm | ≤25 | 7 | 8 |
| Magnesium (Mg), ppm | ≤5 | 3 | 2 |
| Aluminum (Al), ppm | ≤10 | 3 | 4 |
| Potassium (K), ppm | ≤50 | 3 | 4 |
| Calcium (Ca), ppm | ≤50 | 3 | 4 |
| Ferrum (Fe), ppm | ≤3 | 2 | 3 |
| Heavy metal (in Pb), ppm | ≤5 | 2 | 3 |
The natrium carbonicum calcinatum utilizing the present invention to prepare detecting the instrument used: cation adopts plasma mass spectrometry (ICP-MS), anion adopts ionic liquid phase chromatograph (IC), and moisture adopts karl Fischer moisture test apparatus。
As seen from the above table, the purity of the natrium carbonicum calcinatum 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 chemical reagent natrium carbonicum calcinatum pure standard of GBT639-2008 top grade。
Above example is only in order to illustrate technical scheme and on-fixed。Although the present invention having been illustrated with reference to fixing embodiment, the those skilled in the art of the industry are understood that, the technical scheme of invention is modified or replaced on an equal basis, and without deviating from the scope of technical solution of the present invention, it should be included in scope of the presently claimed invention。
Claims (2)
1. a method of purification for technical grade sodium carbonate, comprises the steps:
200g industry natrium carbonicum calcinatum is dissolved at normal temperatures 600mL than the resistance high purity water more than 18M Ω .cm, add 20g polyaluminium hydroxychloride adsorbent, stir 0.5 and little be heated to 48 DEG C at present, insulation stands 1 hour, filtered while hot removes colloid solid phase, membrane filtration is carried out by the acetyl cellulose micropore filtering film in 0.22 μm of aperture under the filtrate insulation obtained, the filtrate obtained concentrates, after removing 120mL water, cool to 3 DEG C, precipitate out crystal, this crystals of sodium carbonate is melted, then under 80 DEG C of conditions, carry out recrystallization, leach recrystallization product, the solid being filtrated to get after being washed is calcined in Muffle furnace at 280 DEG C of temperature, pulverize, obtain 160g SILVER REAGENT natrium carbonicum calcinatum。
2. a method of purification for technical grade sodium carbonate, comprises the steps:
100g industry natrium carbonicum calcinatum is dissolved at normal temperatures 500mL than the resistance high purity water more than 18M Ω .cm, add 10g polyaluminium hydroxychloride adsorbent, stir 0.5 and little be heated to 50 DEG C at present, insulation stands 1.5 hours, filtered while hot removes colloid solid phase, membrane filtration is carried out by the acetyl cellulose micropore filtering film in 0.1 μm of aperture under the filtrate insulation obtained, the filtrate obtained concentrates, after removing 250mL water, cool to 1 DEG C, precipitate out crystal, this crystals of sodium carbonate is melted, then under 90 DEG C of conditions, carry out recrystallization, leach recrystallization product, the solid being filtrated to get after being washed is calcined in Muffle furnace at 300 DEG C of temperature, pulverize, obtain 80g SILVER REAGENT natrium carbonicum calcinatum。
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| 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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| US4288419A (en) * | 1980-04-04 | 1981-09-08 | Intermountain Research & Develop. Corp. | Enhanced recovery of sodium carbonate from NaCl-containing sodium carbonate solutions |
| CN101700897B (en) * | 2009-12-08 | 2011-07-27 | 湖南尔康制药股份有限公司 | Pharmaceutical grade anhydrous sodium carbonate and preparation method thereof |
| CN103601220B (en) * | 2013-12-02 | 2016-01-27 | 国药集团化学试剂有限公司 | A kind of preparation method of SILVER REAGENT anhydrous sodium carbonate |
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