CN104445290A - Method for preparing high-purity anhydrous sodium carbonate by using membrane method - Google Patents
Method for preparing high-purity anhydrous sodium carbonate by using membrane method Download PDFInfo
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- CN104445290A CN104445290A CN201410749553.7A CN201410749553A CN104445290A CN 104445290 A CN104445290 A CN 104445290A CN 201410749553 A CN201410749553 A CN 201410749553A CN 104445290 A CN104445290 A CN 104445290A
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Abstract
The invention discloses a method for preparing high-purity anhydrous sodium carbonate by using a membrane method. The method comprises the following steps: (1) dissolving industrial sodium carbonate with distilled water of 55-65 DEG C, and stirring to ensure that calcium impurities in the industrial sodium carbonate are fully deposited; (2) adding a sodium hydroxide solution into the solution, and stirring at 55-65 DEG C to ensure that magnesium ions in the solution are fully deposited until the magnesium ion content of the solution is lower than 5ppm; (3) filtering the solution by using a ceramic membrane; (4) evaporating a filtrate after filtration, putting an obtained magma solution into a centrifuge for separation, and adding deionized water into the centrifuge to wash filter cakes until no chloride ion is generated in the filter cakes; and (5) drying the product obtained by centrifuging to obtain high-purity anhydrous sodium carbonate, wherein in the high-purity anhydrous sodium carbonate, Ca<2+> is less than or equal to 1ppm, Mg<2+> is less than or equal to 1ppm, SS is less than or equal to 1ppm, and Cl<-> is less than or equal to 2ppm. In the high-purity anhydrous sodium carbonate prepared by the method disclosed by the invention, Ca<2+> is less than or equal to 1ppm, Mg<2+> is less than or equal to 1ppm, SS is less than or equal to 1ppm, and Cl<-> is less than or equal to 2ppm.
Description
Technical field
The present invention relates to a kind of preparation method of high-pure anhydrous sodium carbonate, especially a kind of method using embrane method to prepare high-pure anhydrous sodium carbonate.
Background technology
High-pure anhydrous sodium carbonate can be prepared by industrial sodium carbonate, containing Ca in industrial sodium carbonate
2+, Mg
2+deng impurity, during choline, these foreign ions can be dissolved in mother liquor, need these foreign ions to remove when preparing high-pure anhydrous sodium carbonate, and guarantee obtains qualified high pure sodium carbonate product.Tradition is prepared in high-pure anhydrous sodium carbonate method, for Ca
2+, Mg
2+the removal of impurity, adds sodium hydroxide after choline, adds flocculation agent, uses settling tank to allow precipitation carry out sedimentation, is evaporated by supernatant liquid, centrifugal, washing, drying obtains high-pure anhydrous sodium carbonate product.The method uses settling tank to remove impurity, has floor space comparatively large, and can not realize continuous prodution, the problem that the production cycle is longer.
The patent No. be 200710059570.8 Chinese patent disclose " a kind of low-phosphorous, boron high-pure anhydrous sodium carbonate and preparation method thereof ", the method comprises the following steps: edible soda ash, impurity mass percentage purifying waste water below 0.01%, the caustic soda of mass percentage more than 99% join in material tank and fully react at the temperature of 80--105 DEG C and normal pressure, stir by (a), the choline concentration of described edible soda ash is 360--400 grams per liter, and the add-on of described caustic soda is 50--80 kg/tonne of edible soda ash; B reacted material to be delivered in insulation settling tank with pump and is reacted further by (), the temperature of described settling tank is 60--80 DEG C; C () enters hay tank from the clear liquid that settling tank is extracted out and filters, the filtrate after filtration flows automatically in filtrate tank; D clear liquid in described filtrate tank is got to vaporizer with pump and is evaporated by (), the pressure-controlling of vaporizer at 0.4MPa-0.6MPa, discharging when evaporator temperature is 100--105 DEG C of precipitation to be crystallized and reaches the volume solid-to-liquid ratio of 40%-60%; E () rinses sending into whizzer water from vaporizer material out and carries out solid-liquid separation; F the solid separated from described whizzer is sent into drying bed by (), carry out dry materials, and dried material dosing packaging is finished product, and the bed temperature of described drying bed is 105--150 DEG C, and drying bed intake pressure is 0.8MPa-1.0MPa.The method filtration procedure needs to use settling tank and hay tank, and flow process is more numerous and diverse, and floor space is comparatively large, and products obtained therefrom purity is lower.
The patent No. is that the Chinese patent of CN200810151994.1 discloses " preparation method of anhydrous sodium carbonate ", and method is as follows: (1) makes industrial carbonic acid sodium water solution by water-soluble for industrial sodium carbonate, adds sodium hydroxide removing Mg
2+, Ca
2+; (2) Mg is being removed
2+, Ca
2+hydrogen peroxide is added, removing Fe in aqueous sodium carbonate
2+; (3) to removing Fe
2+cO is passed in aqueous sodium carbonate
2; (4) suction strainer sodium bicarbonate aqueous solution, obtains sodium bicarbonate crystallization; (5) by after sodium bicarbonate crystallization washing, dehydration, drying, standard reagent anhydrous sodium carbonate finished product is obtained.The method needs to carry out carbonization after removal of impurities, and generate sodium bicarbonate, reheat and be decomposed into sodium carbonate, process is more complicated, and the more difficult control of processing condition, cost is higher.
The patent No. is that the Chinese patent of CN201310632706.5 discloses " a kind of preparation method of SILVER REAGENT anhydrous sodium carbonate ", method is as follows: with industrial anhydrous sodium carbonate for raw material, be dissolved in high purity water, add organic amine solid-carried catalyst, then pass into carbon dioxide adjust ph, will the filtrate that obtains be filtered through acetyl cellulose millipore filtration membrane filtration, crystallization, drying, obtains SILVER REAGENT anhydrous sodium carbonate.The acetyl cellulose micropore filtering film alkali resistance that the method prepares the use of high pure sodium carbonate process is poor, and the concentration of sodium carbonate of preparation is lower, and make output in this technique same time lower, suitability for industrialized production economic benefit is poor.
Summary of the invention
The object of the invention is to the shortcoming overcoming prior art, provide one to realize continuous prodution, and the higher a kind of embrane method of the product purity obtained prepares the method for high-pure anhydrous sodium carbonate.
The present invention seeks to be achieved through the following technical solutions.
Embrane method prepares a method for high-pure anhydrous sodium carbonate, and it comprises the following steps:
(1) used by industrial sodium carbonate 55 DEG C of-65 DEG C of distilled water dissolve and stir, the calcium impurities in industrial sodium carbonate is fully precipitated;
(2) add sodium hydroxide solution in the solution, 55 DEG C of-65 DEG C of stirrings, magnesium ion in solution fully precipitated, until in solution magnesium ion content lower than 5ppm;
(3) ceramic membrane is used to filter solution;
(4) by the filtrate evaporation after filtration, the magma obtained is sent into whizzer and is separated, and adds deionized water wash filter cake in centrifuges, until without chlorion in filter cake;
(5) by the centrifugal product drying obtained, high-pure anhydrous sodium carbonate is obtained, Ca in high-pure anhydrous sodium carbonate
2+≤ 1ppm, Mg
2+≤ 1ppm, SS≤1ppm, Cl
-≤ 2ppm.
The present invention has the following advantages: adopt the present invention to carry out the preparation of high-pure anhydrous sodium carbonate, equipment is simple, without the need to secondary carbonization, easy handling, can not large, the high in cost of production problem of continuous prodution, floor space in high pure sodium carbonate preparation technology before overcoming, this technique uses ceramic membrane to filter simultaneously, this film has the advantages that good filtration effect, erosion resistance are strong, life cycle is long, solve the problems such as the production cost that other films cause because of corrosion-resistant is high, productive rate is low, Ca in the high-pure anhydrous sodium carbonate adopting present method obtained
2+≤ 1ppm, Mg
2+≤ 1ppm, SS≤1ppm, Cl
-≤ 2ppm.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
A kind of embrane method of the present invention prepares the method for high-pure anhydrous sodium carbonate, and it comprises the following steps: industrial sodium carbonate uses 55 DEG C of-65 DEG C of distilled water dissolve and stir by (1), and the calcium impurities in industrial sodium carbonate is fully precipitated; (2) add sodium hydroxide solution in the solution, 55 DEG C of-65 DEG C of stirrings, magnesium ion in solution fully precipitated, until in solution magnesium ion content lower than 5ppm; (3) ceramic membrane is used to filter solution; (4) by the filtrate evaporation after filtration, the magma obtained is sent into whizzer and is separated, and adds deionized water wash filter cake in centrifuges, until without chlorion in filter cake; (5) by the centrifugal product drying obtained, high-pure anhydrous sodium carbonate is obtained, Ca in high-pure anhydrous sodium carbonate
2+≤ 1ppm, Mg
2+≤ 1ppm, SS≤1ppm, Cl
-≤ 2ppm.
Embodiment 1
(1) 20kg industrial sodium carbonate is dissolved in 55 DEG C of distilled water and makes the solution that sodium carbonate mass content is about 28%, heated and stirred 1 hour, makes calcium ion fully precipitate;
(2) add sodium hydroxide 20g in the solution, 55 DEG C stir 1 hour, magnesium ion in solution is fully precipitated, until in solution magnesium ion content lower than 5ppm;
(3) use ceramic membrane to filter, obtain refined soln heating evaporation, magma sends into whizzer, and adds deionized water wash filter cake in centrifuges, until without chlorion in filter cake, 110 DEG C of dryings, obtains high pure sodium carbonate.
After tested: in the sodium carbonate using present method to obtain, calcium contents is lower than 1ppm, and Mg content is lower than 1ppm, SS lower than 1ppm, and cl content is lower than 2ppm.
Embodiment 2
(1) 50kg anhydrous sodium carbonate is dissolved in 65 DEG C of distilled water water and prepares the solution that sodium carbonate mass content is about 30%, heated and stirred 1 hour, makes calcium ion fully precipitate;
(2) add sodium hydroxide 50g in the solution, within 1 hour, make magnesium ion in solution fully precipitate 65 DEG C of stirrings, until in solution magnesium ion content lower than 5ppm;
(3) use ceramic membrane to filter, obtain refined soln heating evaporation, magma sends into whizzer, and adds deionized water wash filter cake in centrifuges, until without chlorion in filter cake, 110 DEG C of dryings, obtains high pure sodium carbonate.
After tested: in the sodium carbonate using present method to obtain, calcium contents is lower than 1ppm, Mg content lower than 1ppm, SS≤1ppm, and cl content is lower than 2ppm.
Embodiment 3
(1) 50kg anhydrous sodium carbonate is dissolved in 60 DEG C of distilled water water and prepares the solution that sodium carbonate mass content is about 30%, heated and stirred 1 hour, makes calcium ion fully precipitate;
(2) add sodium hydroxide 50g in the solution, within 1 hour, make magnesium ion in solution fully precipitate 60 DEG C of stirrings, until in solution magnesium ion content lower than 5ppm;
(3) use ceramic membrane to filter, obtain refined soln heating evaporation, magma sends into whizzer, and adds deionized water wash filter cake in centrifuges, until without chlorion in filter cake, 110 DEG C of dryings, obtains high pure sodium carbonate.
After tested: to use in the sodium carbonate that obtains of present method calcium contents lower than 1ppm, Mg content lower than 1ppm, SS≤1ppm, cl content lower than 2ppm.
Claims (1)
1. embrane method prepares a method for high-pure anhydrous sodium carbonate, it is characterized in that it comprises the following steps:
(1) used by industrial sodium carbonate 55 DEG C of-65 DEG C of distilled water dissolve and stir, the calcium impurities in industrial sodium carbonate is fully precipitated;
(2) add sodium hydroxide solution in the solution, 55 DEG C of-65 DEG C of stirrings, magnesium ion in solution fully precipitated, until in solution magnesium ion content lower than 5ppm;
(3) ceramic membrane is used to filter solution;
(4) by the filtrate evaporation after filtration, the magma obtained is sent into whizzer and is separated, and adds deionized water wash filter cake in centrifuges, until without chlorion in filter cake;
(5) by the centrifugal product drying obtained, high-pure anhydrous sodium carbonate is obtained, Ca in high-pure anhydrous sodium carbonate
2+≤ 1ppm, Mg
2+≤ 1ppm, SS≤1ppm, Cl
-≤ 2ppm.
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Cited By (6)
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|---|---|---|---|---|
| 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 |
| CN115676854A (en) * | 2022-09-08 | 2023-02-03 | 西安交通大学 | Method for jointly preparing battery-grade sodium carbonate and basic magnesium carbonate in soda ash industry |
| CN115744934A (en) * | 2022-11-29 | 2023-03-07 | 福建省龙德新能源有限公司 | Preparation method for producing electronic-grade sodium fluoride by purifying industrial-grade sodium carbonate |
| CN115893449A (en) * | 2022-11-29 | 2023-04-04 | 福建省龙德新能源有限公司 | Method for producing electronic-grade sodium fluoride from industrial-grade sodium-alkali mixed liquor |
| CN116443898A (en) * | 2022-11-11 | 2023-07-18 | 唐山三友化工股份有限公司 | Method for preparing battery grade sodium carbonate from industrial sodium carbonate |
| CN117105246A (en) * | 2023-09-26 | 2023-11-24 | 福建省龙德新能源有限公司 | Synthesis process of electronic grade sodium carbonate |
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| CN116443898A (en) * | 2022-11-11 | 2023-07-18 | 唐山三友化工股份有限公司 | Method for preparing battery grade sodium carbonate from industrial sodium carbonate |
| CN116443898B (en) * | 2022-11-11 | 2024-05-10 | 唐山三友化工股份有限公司 | Method for preparing battery grade sodium carbonate from industrial sodium carbonate |
| CN115744934A (en) * | 2022-11-29 | 2023-03-07 | 福建省龙德新能源有限公司 | Preparation method for producing electronic-grade sodium fluoride by purifying industrial-grade sodium carbonate |
| CN115893449A (en) * | 2022-11-29 | 2023-04-04 | 福建省龙德新能源有限公司 | Method for producing electronic-grade sodium fluoride from industrial-grade sodium-alkali mixed liquor |
| CN115893449B (en) * | 2022-11-29 | 2023-08-29 | 福建省龙德新能源有限公司 | Method for producing electronic grade sodium fluoride by using industrial grade sodium-alkali mixed solution |
| CN115744934B (en) * | 2022-11-29 | 2024-03-22 | 福建省龙德新能源有限公司 | Preparation method for producing electronic grade sodium fluoride by purifying industrial grade sodium carbonate |
| CN117105246A (en) * | 2023-09-26 | 2023-11-24 | 福建省龙德新能源有限公司 | Synthesis process of electronic grade sodium carbonate |
| CN117105246B (en) * | 2023-09-26 | 2024-03-29 | 福建省龙德新能源有限公司 | Synthesis process of electronic grade sodium carbonate |
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Application publication date: 20150325 |